# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2014

#===================================================================
data_global
#===================================================================

# SUBMISSION DETAILS
loop_
_publ_contact_author_name     'Dr. Hui-Zhong Kou'
_publ_contact_author_address
;
Department of Chemistry
Tsinghua University
Beijing 100084
People's Republic of China
;
_publ_contact_author_email     'kouhz@mail.tsinghua.edu.cn'
_publ_contact_author_Phone     '86-10-62771748'

_publ_requested_journal        'New J. Chem.'
_publ_requested_category        FM
_publ_requested_coeditor_name    ?
_publ_contact_letter
;
;

# start Validation Reply Form
_vrf_PLAT341_2
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............     0.0187 Ang.  
RESPONSE: This is due to the quality of the diffraction data.
;
_vrf_PLAT043_3
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      12.14 Check 
RESPONSE: The hydrogen atoms of the methanol molecules were not found,
and therefore the molecular formula is different from that calculated
from the ins file.
;
# end Validation Reply Form

#======================================================================   
 
data_1 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C27 H33 Br3 Cl N9 Ni2 O7' 
_chemical_formula_weight          988.22 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ni'  'Ni'   0.3393   1.1124 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.2901   2.4595 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Orthorhombic 
_symmetry_space_group_name_H-M    P2(1)2(1)2(1)
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x+1/2, -y, z+1/2' 
 '-x, y+1/2, -z+1/2' 
 'x+1/2, -y+1/2, -z' 
 
_cell_length_a                    11.763(2) 
_cell_length_b                    12.496(3) 
_cell_length_c                    23.866(5) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.00 
_cell_angle_gamma                 90.00 
_cell_volume                      3508.2(12) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     26531 
_cell_measurement_theta_min       3.04 
_cell_measurement_theta_max       27.47 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             'red brown' 
_exptl_crystal_size_max           0.18 
_exptl_crystal_size_mid           0.16 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.871 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1968 
_exptl_absorpt_coefficient_mu     4.624 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.460 
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    'ABSCOR; T Higashi (2001)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku R-AXIS RAPID IP' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  0.77 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             34383 
_diffrn_reflns_av_R_equivalents   0.0585 
_diffrn_reflns_av_sigmaI/netI     0.0526 
_diffrn_reflns_limit_h_min        -15 
_diffrn_reflns_limit_h_max        15 
_diffrn_reflns_limit_k_min        -16 
_diffrn_reflns_limit_k_max        16 
_diffrn_reflns_limit_l_min        -30 
_diffrn_reflns_limit_l_max        30 
_diffrn_reflns_theta_min          3.04 
_diffrn_reflns_theta_max          27.47 
_reflns_number_total              8007 
_reflns_number_gt                 6184 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_cell_refinement        'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_reduction         'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'XP (Sheldrick, 1998)' 
_computing_publication_material   'XP (Sheldrick, 1998)' 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0479P)²+3.5674P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ?
_chemical_absolute_configuration  UNK
_refine_ls_abs_structure_details 
 'Flack H D (1983), Acta Cryst. A39, 876-881' 
_refine_ls_abs_structure_Flack    0.051(11) 
_refine_ls_number_reflns          8007 
_refine_ls_number_parameters      442 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0626 
_refine_ls_R_factor_gt            0.0372 
_refine_ls_wR_factor_ref          0.1109 
_refine_ls_wR_factor_gt           0.0827 
_refine_ls_goodness_of_fit_ref    1.074 
_refine_ls_restrained_S_all       1.074 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ni1 Ni 0.93921(4) 0.06545(4) 0.90378(2) 0.02990(12) Uani 1 1 d . . . 
Ni2 Ni 1.16087(4) -0.12343(4) 0.91117(2) 0.02919(12) Uani 1 1 d . . . 
Br3 Br 0.86283(4) 0.35583(4) 0.94662(2) 0.05238(13) Uani 1 1 d . . . 
O3 O 1.1053(2) -0.0606(2) 0.83580(11) 0.0343(7) Uani 1 1 d . . . 
N8 N 1.0659(3) 0.0626(3) 0.96143(13) 0.0311(8) Uani 1 1 d . . . 
N7 N 0.9207(3) -0.0944(3) 0.90931(14) 0.0323(8) Uani 1 1 d . . . 
O2 O 1.1685(2) 0.0245(2) 0.94950(12) 0.0345(7) Uani 1 1 d . . . 
N6 N 1.0568(3) 0.0344(3) 0.84264(14) 0.0318(8) Uani 1 1 d . . . 
O1 O 0.9952(2) -0.1558(2) 0.93681(12) 0.0358(7) Uani 1 1 d . . . 
N5 N 1.3338(3) -0.1083(3) 0.88826(15) 0.0373(9) Uani 1 1 d . . . 
C25 C 0.7174(3) 0.0884(4) 0.81144(18) 0.0374(10) Uani 1 1 d . . . 
N4 N 1.1785(3) -0.2790(3) 0.87504(15) 0.0388(9) Uani 1 1 d . . . 
C24 C 0.7728(3) -0.0753(4) 0.84343(17) 0.0343(10) Uani 1 1 d . . . 
N3 N 1.2288(3) -0.2003(3) 0.98316(15) 0.0385(9) Uani 1 1 d . . . 
N2 N 0.7885(3) 0.0331(3) 0.84431(14) 0.0312(8) Uani 1 1 d . . . 
C23 C 0.6341(4) 0.0453(4) 0.77691(19) 0.0435(12) Uani 1 1 d . . . 
H23A H 0.5873 0.0890 0.7553 0.052 Uiso 1 1 calc R . . 
C22 C 0.8464(3) -0.1406(4) 0.87799(16) 0.0324(10) Uani 1 1 d . . . 
H22A H 0.8400 -0.2147 0.8776 0.039 Uiso 1 1 calc R . . 
C21 C 1.0388(3) 0.2163(4) 0.82043(18) 0.0356(10) Uani 1 1 d . . . 
C20 C 0.6233(4) -0.0629(5) 0.7758(2) 0.0490(13) Uani 1 1 d . . . 
H20A H 0.5701 -0.0950 0.7524 0.059 Uiso 1 1 calc R . . 
C19 C 0.6924(4) -0.1252(4) 0.80976(19) 0.0429(12) Uani 1 1 d . . . 
H19A H 0.6850 -0.1993 0.8100 0.051 Uiso 1 1 calc R . . 
C18 C 1.0838(4) 0.1102(4) 0.80875(18) 0.0364(10) Uani 1 1 d . . . 
H18A H 1.1304 0.0977 0.7780 0.044 Uiso 1 1 calc R . . 
C17 C 1.2373(5) -0.3168(4) 0.9729(2) 0.0513(14) Uani 1 1 d . . . 
H17A H 1.2138 -0.3551 1.0063 0.062 Uiso 1 1 calc R . . 
H17B H 1.3160 -0.3352 0.9654 0.062 Uiso 1 1 calc R . . 
N1 N 0.8492(3) 0.1069(3) 0.98480(14) 0.0349(9) Uani 1 1 d . . . 
N9 N 0.9772(3) 0.2300(3) 0.86855(14) 0.0339(9) Uani 1 1 d . . . 
C15 C 1.1652(5) -0.3519(4) 0.9245(2) 0.0512(13) Uani 1 1 d . . . 
H15A H 1.1864 -0.4240 0.9137 0.061 Uiso 1 1 calc R . . 
H15B H 1.0861 -0.3529 0.9359 0.061 Uiso 1 1 calc R . . 
C14 C 1.4057(4) -0.1471(5) 0.9347(2) 0.0553(15) Uani 1 1 d . . . 
H14A H 1.4716 -0.1010 0.9382 0.066 Uiso 1 1 calc R . . 
H14B H 1.4325 -0.2186 0.9260 0.066 Uiso 1 1 calc R . . 
C13 C 1.1595(5) -0.1778(5) 1.03289(19) 0.0531(14) Uani 1 1 d . . . 
H13A H 1.1917 -0.2133 1.0648 0.080 Uiso 1 1 calc R . . 
H13B H 1.0834 -0.2033 1.0269 0.080 Uiso 1 1 calc R . . 
H13C H 1.1578 -0.1021 1.0395 0.080 Uiso 1 1 calc R . . 
C12 C 0.7434(4) 0.1297(4) 1.0000(2) 0.0430(12) Uani 1 1 d . . . 
C11 C 1.2929(4) -0.2866(4) 0.8493(2) 0.0510(13) Uani 1 1 d . . . 
H11A H 1.2877 -0.3266 0.8146 0.061 Uiso 1 1 calc R . . 
H11B H 1.3430 -0.3255 0.8744 0.061 Uiso 1 1 calc R . . 
C10 C 1.0164(5) 0.4002(5) 0.7948(2) 0.0596(15) Uani 1 1 d . . . 
H10A H 1.0267 0.4560 0.7695 0.072 Uiso 1 1 calc R . . 
C9 C 1.3428(4) -0.1494(4) 0.9894(2) 0.0494(13) Uani 1 1 d . . . 
H9A H 1.3870 -0.1889 1.0168 0.059 Uiso 1 1 calc R . . 
H9B H 1.3336 -0.0768 1.0031 0.059 Uiso 1 1 calc R . . 
C8 C 1.3427(4) -0.1792(4) 0.8376(2) 0.0515(14) Uani 1 1 d . . . 
H8A H 1.3028 -0.1464 0.8064 0.062 Uiso 1 1 calc R . . 
H8B H 1.4219 -0.1871 0.8271 0.062 Uiso 1 1 calc R . . 
C7 C 1.0595(4) 0.2989(4) 0.7833(2) 0.0489(13) Uani 1 1 d . . . 
H7A H 1.1018 0.2868 0.7510 0.059 Uiso 1 1 calc R . . 
C6 C 1.3628(4) 0.0029(4) 0.8722(2) 0.0460(12) Uani 1 1 d . . . 
H6A H 1.4417 0.0066 0.8620 0.069 Uiso 1 1 calc R . . 
H6B H 1.3486 0.0499 0.9032 0.069 Uiso 1 1 calc R . . 
H6C H 1.3169 0.0243 0.8409 0.069 Uiso 1 1 calc R . . 
C5 C 0.9289(4) 0.1245(4) 1.02494(19) 0.0437(12) Uani 1 1 d . . . 
C4 C 0.9420(4) 0.3286(4) 0.8787(2) 0.0403(11) Uani 1 1 d . . . 
C3 C 0.7936(5) 0.1954(6) 1.0894(3) 0.0706(18) Uani 1 1 d . . . 
H3A H 0.7754 0.2264 1.1236 0.085 Uiso 1 1 calc R . . 
C2 C 0.7102(4) 0.1755(5) 1.0498(3) 0.0618(16) Uani 1 1 d . . . 
H2A H 0.6345 0.1926 1.0566 0.074 Uiso 1 1 calc R . . 
C1 C 0.9045(5) 0.1679(5) 1.0767(2) 0.0597(17) Uani 1 1 d . . . 
H1A H 0.9621 0.1786 1.1029 0.072 Uiso 1 1 calc R . . 
Cl1 Cl 0.65072(11) 0.56093(11) 0.81734(6) 0.0568(3) Uani 1 1 d . . . 
C26 C 0.9586(4) 0.4163(4) 0.8438(2) 0.0504(13) Uani 1 1 d . . . 
H26A H 0.9312 0.4836 0.8534 0.061 Uiso 1 1 calc R . . 
C27 C 1.0457(4) 0.0965(4) 1.01155(18) 0.0398(11) Uani 1 1 d . . . 
H27A H 1.1035 0.1028 1.0380 0.048 Uiso 1 1 calc R . . 
C28 C 1.0900(4) -0.3019(5) 0.8337(2) 0.0514(14) Uani 1 1 d . . . 
H28A H 1.1012 -0.3724 0.8187 0.077 Uiso 1 1 calc R . . 
H28B H 1.0941 -0.2504 0.8039 0.077 Uiso 1 1 calc R . . 
H28C H 1.0168 -0.2978 0.8513 0.077 Uiso 1 1 calc R . . 
O4 O 0.7577(4) 0.6093(4) 0.8280(2) 0.0907(16) Uani 1 1 d . . . 
O5 O 0.5627(4) 0.6265(5) 0.8329(3) 0.135(2) Uani 1 1 d . . . 
O6 O 0.6445(6) 0.5112(9) 0.7692(3) 0.224(4) Uani 1 1 d . . . 
O7 O 0.6455(9) 0.4760(6) 0.8582(4) 0.193(4) Uani 1 1 d . . . 
Br1 Br 0.62559(4) 0.09776(5) 0.94827(2) 0.06219(17) Uani 1 1 d . . . 
Br2 Br 0.72011(4) 0.23977(4) 0.81496(2) 0.05430(14) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Ni1 N7 2.013(4) . ? 
Ni1 N8 2.029(3) . ? 
Ni1 N6 2.047(3) . ? 
Ni1 N1 2.265(3) . ? 
Ni1 N9 2.266(4) . ? 
Ni1 N2 2.307(3) . ? 
Ni2 O2 2.065(3) . ? 
Ni2 O3 2.069(3) . ? 
Ni2 O1 2.082(3) . ? 
Ni2 N5 2.115(3) . ? 
Ni2 N3 2.125(4) . ? 
Ni2 N4 2.137(4) . ? 
Br3 C4 1.899(5) . ? 
O3 N6 1.328(5) . ? 
N8 C27 1.291(5) . ? 
N8 O2 1.328(4) . ? 
N7 C22 1.287(5) . ? 
N7 O1 1.337(4) . ? 
N6 C18 1.285(5) . ? 
N5 C14 1.476(6) . ? 
N5 C6 1.482(6) . ? 
N5 C8 1.503(6) . ? 
C25 N2 1.339(5) . ? 
C25 C23 1.389(6) . ? 
C25 Br2 1.894(4) . ? 
N4 C28 1.463(6) . ? 
N4 C11 1.482(6) . ? 
N4 C15 1.498(6) . ? 
C24 N2 1.367(6) . ? 
C24 C19 1.389(6) . ? 
C24 C22 1.447(6) . ? 
N3 C13 1.467(6) . ? 
N3 C17 1.480(7) . ? 
N3 C9 1.492(6) . ? 
C23 C20 1.359(7) . ? 
C23 H23A 0.9300 . ? 
C22 H22A 0.9300 . ? 
C21 N9 1.368(5) . ? 
C21 C7 1.381(6) . ? 
C21 C18 1.455(6) . ? 
C20 C19 1.387(7) . ? 
C20 H20A 0.9300 . ? 
C19 H19A 0.9300 . ? 
C18 H18A 0.9300 . ? 
C17 C15 1.499(7) . ? 
C17 H17A 0.9700 . ? 
C17 H17B 0.9700 . ? 
N1 C12 1.327(5) . ? 
N1 C5 1.358(6) . ? 
N9 C4 1.322(6) . ? 
C15 H15A 0.9700 . ? 
C15 H15B 0.9700 . ? 
C14 C9 1.501(7) . ? 
C14 H14A 0.9700 . ? 
C14 H14B 0.9700 . ? 
C13 H13A 0.9600 . ? 
C13 H13B 0.9600 . ? 
C13 H13C 0.9600 . ? 
C12 C2 1.375(7) . ? 
C12 Br1 1.898(5) . ? 
C11 C8 1.491(8) . ? 
C11 H11A 0.9700 . ? 
C11 H11B 0.9700 . ? 
C10 C26 1.368(8) . ? 
C10 C7 1.391(8) . ? 
C10 H10A 0.9300 . ? 
C9 H9A 0.9700 . ? 
C9 H9B 0.9700 . ? 
C8 H8A 0.9700 . ? 
C8 H8B 0.9700 . ? 
C7 H7A 0.9300 . ? 
C6 H6A 0.9600 . ? 
C6 H6B 0.9600 . ? 
C6 H6C 0.9600 . ? 
C5 C1 1.380(7) . ? 
C5 C27 1.454(6) . ? 
C4 C26 1.390(7) . ? 
C3 C1 1.382(8) . ? 
C3 C2 1.384(8) . ? 
C3 H3A 0.9300 . ? 
C2 H2A 0.9300 . ? 
C1 H1A 0.9300 . ? 
Cl1 O6 1.309(7) . ? 
Cl1 O5 1.372(5) . ? 
Cl1 O4 1.420(5) . ? 
Cl1 O7 1.443(7) . ? 
C26 H26A 0.9300 . ? 
C27 H27A 0.9300 . ? 
C28 H28A 0.9600 . ? 
C28 H28B 0.9600 . ? 
C28 H28C 0.9600 . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N7 Ni1 N8 91.01(14) . . ? 
N7 Ni1 N6 86.10(14) . . ? 
N8 Ni1 N6 89.08(13) . . ? 
N7 Ni1 N1 96.91(14) . . ? 
N8 Ni1 N1 76.61(12) . . ? 
N6 Ni1 N1 165.39(13) . . ? 
N7 Ni1 N9 161.05(14) . . ? 
N8 Ni1 N9 97.02(13) . . ? 
N6 Ni1 N9 76.94(13) . . ? 
N1 Ni1 N9 101.63(13) . . ? 
N7 Ni1 N2 77.48(13) . . ? 
N8 Ni1 N2 168.20(14) . . ? 
N6 Ni1 N2 92.72(13) . . ? 
N1 Ni1 N2 101.89(12) . . ? 
N9 Ni1 N2 94.74(12) . . ? 
O2 Ni2 O3 93.38(12) . . ? 
O2 Ni2 O1 94.83(11) . . ? 
O3 Ni2 O1 91.91(11) . . ? 
O2 Ni2 N5 89.59(13) . . ? 
O3 Ni2 N5 92.58(13) . . ? 
O1 Ni2 N5 173.50(14) . . ? 
O2 Ni2 N3 91.75(14) . . ? 
O3 Ni2 N3 173.56(13) . . ? 
O1 Ni2 N3 91.53(13) . . ? 
N5 Ni2 N3 83.56(14) . . ? 
O2 Ni2 N4 171.59(12) . . ? 
O3 Ni2 N4 91.45(13) . . ? 
O1 Ni2 N4 91.89(13) . . ? 
N5 Ni2 N4 83.31(14) . . ? 
N3 Ni2 N4 83.00(15) . . ? 
N6 O3 Ni2 111.6(2) . . ? 
C27 N8 O2 118.9(3) . . ? 
C27 N8 Ni1 119.2(3) . . ? 
O2 N8 Ni1 121.9(2) . . ? 
C22 N7 O1 118.2(4) . . ? 
C22 N7 Ni1 118.7(3) . . ? 
O1 N7 Ni1 122.1(2) . . ? 
N8 O2 Ni2 112.1(2) . . ? 
C18 N6 O3 118.3(3) . . ? 
C18 N6 Ni1 118.5(3) . . ? 
O3 N6 Ni1 123.2(2) . . ? 
N7 O1 Ni2 111.0(2) . . ? 
C14 N5 C6 111.8(4) . . ? 
C14 N5 C8 111.7(4) . . ? 
C6 N5 C8 109.2(4) . . ? 
C14 N5 Ni2 109.1(3) . . ? 
C6 N5 Ni2 111.9(3) . . ? 
C8 N5 Ni2 102.9(3) . . ? 
N2 C25 C23 126.0(4) . . ? 
N2 C25 Br2 118.6(3) . . ? 
C23 C25 Br2 115.2(3) . . ? 
C28 N4 C11 110.8(4) . . ? 
C28 N4 C15 109.8(4) . . ? 
C11 N4 C15 112.5(4) . . ? 
C28 N4 Ni2 112.4(3) . . ? 
C11 N4 Ni2 108.2(3) . . ? 
C15 N4 Ni2 103.0(3) . . ? 
N2 C24 C19 123.1(4) . . ? 
N2 C24 C22 117.9(4) . . ? 
C19 C24 C22 118.9(4) . . ? 
C13 N3 C17 111.1(4) . . ? 
C13 N3 C9 109.7(4) . . ? 
C17 N3 C9 112.0(4) . . ? 
C13 N3 Ni2 111.0(3) . . ? 
C17 N3 Ni2 109.7(3) . . ? 
C9 N3 Ni2 103.0(3) . . ? 
C25 N2 C24 114.7(3) . . ? 
C25 N2 Ni1 138.6(3) . . ? 
C24 N2 Ni1 106.7(3) . . ? 
C20 C23 C25 117.6(4) . . ? 
C20 C23 H23A 121.2 . . ? 
C25 C23 H23A 121.2 . . ? 
N7 C22 C24 119.0(4) . . ? 
N7 C22 H22A 120.5 . . ? 
C24 C22 H22A 120.5 . . ? 
N9 C21 C7 122.6(4) . . ? 
N9 C21 C18 117.9(4) . . ? 
C7 C21 C18 119.6(4) . . ? 
C23 C20 C19 119.5(4) . . ? 
C23 C20 H20A 120.2 . . ? 
C19 C20 H20A 120.2 . . ? 
C20 C19 C24 119.0(5) . . ? 
C20 C19 H19A 120.5 . . ? 
C24 C19 H19A 120.5 . . ? 
N6 C18 C21 117.4(4) . . ? 
N6 C18 H18A 121.3 . . ? 
C21 C18 H18A 121.3 . . ? 
N3 C17 C15 112.1(4) . . ? 
N3 C17 H17A 109.2 . . ? 
C15 C17 H17A 109.2 . . ? 
N3 C17 H17B 109.2 . . ? 
C15 C17 H17B 109.2 . . ? 
H17A C17 H17B 107.9 . . ? 
C12 N1 C5 114.8(4) . . ? 
C12 N1 Ni1 136.1(3) . . ? 
C5 N1 Ni1 108.4(3) . . ? 
C4 N9 C21 115.9(4) . . ? 
C4 N9 Ni1 135.7(3) . . ? 
C21 N9 Ni1 107.6(3) . . ? 
N4 C15 C17 111.7(4) . . ? 
N4 C15 H15A 109.3 . . ? 
C17 C15 H15A 109.3 . . ? 
N4 C15 H15B 109.3 . . ? 
C17 C15 H15B 109.3 . . ? 
H15A C15 H15B 107.9 . . ? 
N5 C14 C9 112.1(4) . . ? 
N5 C14 H14A 109.2 . . ? 
C9 C14 H14A 109.2 . . ? 
N5 C14 H14B 109.2 . . ? 
C9 C14 H14B 109.2 . . ? 
H14A C14 H14B 107.9 . . ? 
N3 C13 H13A 109.5 . . ? 
N3 C13 H13B 109.5 . . ? 
H13A C13 H13B 109.5 . . ? 
N3 C13 H13C 109.5 . . ? 
H13A C13 H13C 109.5 . . ? 
H13B C13 H13C 109.5 . . ? 
N1 C12 C2 126.2(5) . . ? 
N1 C12 Br1 117.5(3) . . ? 
C2 C12 Br1 116.3(3) . . ? 
N4 C11 C8 112.2(4) . . ? 
N4 C11 H11A 109.2 . . ? 
C8 C11 H11A 109.2 . . ? 
N4 C11 H11B 109.2 . . ? 
C8 C11 H11B 109.2 . . ? 
H11A C11 H11B 107.9 . . ? 
C26 C10 C7 118.9(5) . . ? 
C26 C10 H10A 120.5 . . ? 
C7 C10 H10A 120.5 . . ? 
N3 C9 C14 111.4(4) . . ? 
N3 C9 H9A 109.4 . . ? 
C14 C9 H9A 109.4 . . ? 
N3 C9 H9B 109.4 . . ? 
C14 C9 H9B 109.4 . . ? 
H9A C9 H9B 108.0 . . ? 
C11 C8 N5 110.6(4) . . ? 
C11 C8 H8A 109.5 . . ? 
N5 C8 H8A 109.5 . . ? 
C11 C8 H8B 109.5 . . ? 
N5 C8 H8B 109.5 . . ? 
H8A C8 H8B 108.1 . . ? 
C21 C7 C10 119.3(5) . . ? 
C21 C7 H7A 120.4 . . ? 
C10 C7 H7A 120.4 . . ? 
N5 C6 H6A 109.5 . . ? 
N5 C6 H6B 109.5 . . ? 
H6A C6 H6B 109.5 . . ? 
N5 C6 H6C 109.5 . . ? 
H6A C6 H6C 109.5 . . ? 
H6B C6 H6C 109.5 . . ? 
N1 C5 C1 123.5(4) . . ? 
N1 C5 C27 117.3(4) . . ? 
C1 C5 C27 119.2(4) . . ? 
N9 C4 C26 125.4(5) . . ? 
N9 C4 Br3 118.5(3) . . ? 
C26 C4 Br3 116.1(4) . . ? 
C1 C3 C2 118.4(5) . . ? 
C1 C3 H3A 120.8 . . ? 
C2 C3 H3A 120.8 . . ? 
C12 C2 C3 117.6(5) . . ? 
C12 C2 H2A 121.2 . . ? 
C3 C2 H2A 121.2 . . ? 
C5 C1 C3 119.3(5) . . ? 
C5 C1 H1A 120.4 . . ? 
C3 C1 H1A 120.4 . . ? 
O6 Cl1 O5 118.6(5) . . ? 
O6 Cl1 O4 114.1(4) . . ? 
O5 Cl1 O4 111.5(3) . . ? 
O6 Cl1 O7 104.0(6) . . ? 
O5 Cl1 O7 103.0(5) . . ? 
O4 Cl1 O7 103.3(5) . . ? 
C10 C26 C4 117.8(5) . . ? 
C10 C26 H26A 121.1 . . ? 
C4 C26 H26A 121.1 . . ? 
N8 C27 C5 117.1(4) . . ? 
N8 C27 H27A 121.4 . . ? 
C5 C27 H27A 121.4 . . ? 
N4 C28 H28A 109.5 . . ? 
N4 C28 H28B 109.5 . . ? 
H28A C28 H28B 109.5 . . ? 
N4 C28 H28C 109.5 . . ? 
H28A C28 H28C 109.5 . . ? 
H28B C28 H28C 109.5 . . ? 
 
_diffrn_measured_fraction_theta_max    0.997 
_diffrn_reflns_theta_full              27.47 
_diffrn_measured_fraction_theta_full   0.997 
_refine_diff_density_max    1.018 
_refine_diff_density_min   -0.791 
_refine_diff_density_rms    0.122 

#===End

data_2 
 
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C27 H33 B Br3 F4 N9 Ni2 O3' 
_chemical_formula_weight          975.58 
 
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Br'  'Br'  -0.2901   2.4595 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'F'  'F'   0.0171   0.0103 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ni'  'Ni'   0.3393   1.1124 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
 
_cell_length_a                    12.5650(6) 
_cell_length_b                    12.2327(8) 
_cell_length_c                    22.9117(12) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.465(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      3515.2(3) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     19810 
_cell_measurement_theta_min       2.99 
_cell_measurement_theta_max       27.46 
 
_exptl_crystal_description        block 
_exptl_crystal_colour             red 
_exptl_crystal_size_max           0.22 
_exptl_crystal_size_mid           0.19 
_exptl_crystal_size_min           0.15 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.843 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              1936 
_exptl_absorpt_coefficient_mu     4.547 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.317 
_exptl_absorpt_correction_T_max   1.0000 
_exptl_absorpt_process_details    'ABSCOR; T Higashi (2001)' 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku R-AXIS RAPID IP' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  0.77 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             26626 
_diffrn_reflns_av_R_equivalents   0.0580 
_diffrn_reflns_av_sigmaI/netI     0.0482 
_diffrn_reflns_limit_h_min        -14 
_diffrn_reflns_limit_h_max        14 
_diffrn_reflns_limit_k_min        -14 
_diffrn_reflns_limit_k_max        14 
_diffrn_reflns_limit_l_min        -27 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          2.99 
_diffrn_reflns_theta_max          25.00 
_reflns_number_total              6156 
_reflns_number_gt                 4431 
_reflns_threshold_expression      >2sigma(I) 
 
_computing_data_collection        'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_cell_refinement        'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_reduction         'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'XP (Sheldrick, 1998)' 
_computing_publication_material   'XP (Sheldrick, 1998)' 
 
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 
_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc  
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0625P)²+53.7301P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      SHELXL 
_refine_ls_extinction_coef        0.0047(4) 
_refine_ls_extinction_expression 
 'Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^' 
_refine_ls_number_reflns          6156 
_refine_ls_number_parameters      474 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0964 
_refine_ls_R_factor_gt            0.0685 
_refine_ls_wR_factor_ref          0.2211 
_refine_ls_wR_factor_gt           0.2004 
_refine_ls_goodness_of_fit_ref    1.115 
_refine_ls_restrained_S_all       1.115 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Br1 Br 0.72851(9) 0.41606(11) 0.06440(6) 0.0575(4) Uani 1 1 d . . . 
Ni1 Ni 0.98633(10) 0.25307(11) 0.09886(6) 0.0383(4) Uani 1 1 d . . . 
Ni2 Ni 1.26680(10) 0.24935(11) 0.10233(6) 0.0393(4) Uani 1 1 d . . . 
O1 O 1.1723(5) 0.1363(6) 0.0560(3) 0.0471(18) Uani 1 1 d . . . 
B1 B 0.5083(13) -0.2443(16) 0.1552(8) 0.068(4) Uani 1 1 d . . . 
F1 F 0.4820(18) -0.206(4) 0.1016(8) 0.106(15) Uani 0.56(4) 1 d P A 1 
F2 F 0.4203(6) -0.2529(8) 0.1865(4) 0.088(3) Uani 1 1 d . A 1 
F3 F 0.560(3) -0.336(3) 0.1574(17) 0.134(15) Uani 0.56(4) 1 d P A 1 
F4 F 0.566(2) -0.162(4) 0.1827(12) 0.130(15) Uani 0.56(4) 1 d P A 1 
F1A F 0.488(5) -0.324(6) 0.107(3) 0.19(3) Uani 0.44(4) 1 d P A 2 
F3A F 0.519(5) -0.159(5) 0.121(4) 0.19(3) Uani 0.44(4) 1 d P A 2 
F4A F 0.613(2) -0.265(5) 0.1774(17) 0.120(16) Uani 0.44(4) 1 d P A 2 
O2 O 1.1803(6) 0.2323(7) 0.1774(3) 0.0473(19) Uani 1 1 d . . . 
N2 N 1.3797(7) 0.3598(9) 0.1403(4) 0.051(2) Uani 1 1 d . . . 
C2 C 0.8884(11) -0.0838(11) 0.1143(6) 0.063(3) Uani 1 1 d . . . 
H2A H 0.9161 -0.1453 0.0968 0.075 Uiso 1 1 calc R . . 
C4 C 1.4688(10) 0.2967(12) 0.1715(6) 0.065(4) Uani 1 1 d . . . 
H4A H 1.5291 0.2927 0.1471 0.078 Uiso 1 1 calc R . . 
H4B H 1.4916 0.3339 0.2075 0.078 Uiso 1 1 calc R . . 
Br5 Br 0.72772(10) 0.11953(12) 0.02539(6) 0.0619(4) Uani 1 1 d . . . 
N5 N 0.9061(7) 0.3945(8) 0.1411(4) 0.041(2) Uani 1 1 d . . . 
Br6 Br 0.76375(11) 0.21710(13) 0.20800(6) 0.0706(5) Uani 1 1 d . . . 
O6 O 1.1759(5) 0.3821(6) 0.0735(3) 0.0453(18) Uani 1 1 d . . . 
N6 N 0.8974(7) 0.2588(7) 0.0071(4) 0.039(2) Uani 1 1 d . . . 
C6 C 0.7690(11) 0.2392(10) -0.0749(6) 0.060(3) Uani 1 1 d . . . 
H6A H 0.7066 0.2062 -0.0901 0.072 Uiso 1 1 calc R . . 
N7 N 1.3753(7) 0.1302(8) 0.1341(4) 0.051(2) Uani 1 1 d . . . 
C7 C 1.4318(10) 0.1844(12) 0.1850(6) 0.063(3) Uani 1 1 d . . . 
H7A H 1.4920 0.1410 0.1973 0.075 Uiso 1 1 d R . . 
H7B H 1.3817 0.1888 0.2140 0.075 Uiso 1 1 d R . . 
N10 N 1.3649(7) 0.2539(8) 0.0308(4) 0.044(2) Uani 1 1 d . . . 
C11 C 0.7581(10) -0.0014(13) 0.1702(5) 0.063(4) Uani 1 1 d . . . 
H11A H 0.6962 -0.0051 0.1905 0.075 Uiso 1 1 calc R . . 
N12 N 0.9006(7) 0.1092(8) 0.1357(4) 0.044(2) Uani 1 1 d . . . 
N13 N 1.0762(7) 0.1238(8) 0.0770(4) 0.043(2) Uani 1 1 d . . . 
C14 C 1.3322(11) 0.4393(13) 0.1793(6) 0.070(4) Uani 1 1 d . . . 
H14A H 1.3835 0.4952 0.1898 0.105 Uiso 1 1 calc R . . 
H14B H 1.3116 0.4028 0.2139 0.105 Uiso 1 1 calc R . . 
H14C H 1.2706 0.4719 0.1595 0.105 Uiso 1 1 calc R . . 
C15 C 0.9394(11) 0.5109(13) 0.2255(6) 0.070(4) Uani 1 1 d . . . 
H15A H 0.9829 0.5292 0.2584 0.084 Uiso 1 1 calc R . . 
N16 N 1.0863(7) 0.2818(8) 0.1696(4) 0.043(2) Uani 1 1 d . . . 
N17 N 1.0787(6) 0.3499(7) 0.0524(4) 0.039(2) Uani 1 1 d . . . 
C17 C 0.9511(9) 0.3309(10) -0.0265(5) 0.044(3) Uani 1 1 d . . . 
C19 C 1.4116(10) 0.1403(11) 0.0295(6) 0.061(3) Uani 1 1 d . . . 
H19A H 1.3573 0.0894 0.0146 0.074 Uiso 1 1 calc R . . 
H19B H 1.4693 0.1392 0.0032 0.074 Uiso 1 1 calc R . . 
C20 C 0.7959(11) -0.0916(12) 0.1441(6) 0.067(4) Uani 1 1 d . . . 
H20A H 0.7602 -0.1579 0.1461 0.081 Uiso 1 1 calc R . . 
C21 C 0.9394(9) 0.0164(10) 0.1108(5) 0.049(3) Uani 1 1 d . . . 
C26 C 0.8228(12) 0.3102(13) -0.1073(6) 0.071(4) Uani 1 1 d . . . 
H26A H 0.7986 0.3269 -0.1454 0.085 Uiso 1 1 calc R . . 
C27 C 1.3024(10) 0.2763(12) -0.0246(5) 0.061(3) Uani 1 1 d . . . 
H27A H 1.3491 0.2774 -0.0562 0.091 Uiso 1 1 calc R . . 
H27B H 1.2677 0.3459 -0.0221 0.091 Uiso 1 1 calc R . . 
H27C H 1.2497 0.2201 -0.0314 0.091 Uiso 1 1 calc R . . 
C28 C 0.9139(11) 0.3572(12) -0.0829(6) 0.066(4) Uani 1 1 d . . . 
H28A H 0.9512 0.4072 -0.1044 0.079 Uiso 1 1 calc R . . 
C29 C 1.4490(10) 0.3350(11) 0.0414(6) 0.061(3) Uani 1 1 d . . . 
H29A H 1.4601 0.3738 0.0054 0.073 Uiso 1 1 calc R . . 
H29B H 1.5150 0.2982 0.0536 0.073 Uiso 1 1 calc R . . 
C31 C 1.0368(9) 0.0277(10) 0.0800(5) 0.049(3) Uani 1 1 d . . . 
H31A H 1.0689 -0.0322 0.0633 0.059 Uiso 1 1 calc R . . 
C34 C 1.4522(11) 0.1049(12) 0.0883(6) 0.066(4) Uani 1 1 d . . . 
H34A H 1.5194 0.1413 0.0982 0.079 Uiso 1 1 calc R . . 
H34B H 1.4654 0.0268 0.0878 0.079 Uiso 1 1 calc R . . 
C36 C 0.8493(13) 0.5688(12) 0.2118(6) 0.075(4) Uani 1 1 d . . . 
H36A H 0.8297 0.6255 0.2359 0.090 Uiso 1 1 calc R . . 
C40 C 1.4211(10) 0.4156(11) 0.0879(6) 0.062(3) Uani 1 1 d . . . 
H40A H 1.4840 0.4578 0.0999 0.075 Uiso 1 1 calc R . . 
H40B H 1.3674 0.4658 0.0716 0.075 Uiso 1 1 calc R . . 
C41 C 1.0482(8) 0.3760(10) -0.0002(5) 0.048(3) Uani 1 1 d . . . 
H41A H 1.0887 0.4239 -0.0213 0.057 Uiso 1 1 calc R . . 
C44 C 0.9663(8) 0.4241(10) 0.1903(5) 0.047(3) Uani 1 1 d . . . 
C45 C 1.0632(9) 0.3584(10) 0.2036(5) 0.050(3) Uani 1 1 d . . . 
H45A H 1.1070 0.3732 0.2368 0.060 Uiso 1 1 calc R . . 
C46 C 0.7878(10) 0.5442(11) 0.1631(6) 0.060(3) Uani 1 1 d . . . 
H46A H 0.7274 0.5850 0.1522 0.072 Uiso 1 1 calc R . . 
C47 C 0.8093(9) 0.2167(10) -0.0185(5) 0.049(3) Uani 1 1 d . . . 
C50 C 0.8187(8) 0.4551(10) 0.1298(5) 0.047(3) Uani 1 1 d . . . 
C51 C 1.3208(11) 0.0288(11) 0.1532(7) 0.073(4) Uani 1 1 d . . . 
H51A H 1.3686 -0.0123 0.1790 0.110 Uiso 1 1 calc R . . 
H51B H 1.3001 -0.0148 0.1195 0.110 Uiso 1 1 calc R . . 
H51C H 1.2586 0.0484 0.1732 0.110 Uiso 1 1 calc R . . 
C53 C 0.8136(9) 0.0978(11) 0.1663(5) 0.051(3) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Br1 C50 1.884(12) . ? 
Ni1 N17 2.009(9) . ? 
Ni1 N16 2.020(9) . ? 
Ni1 N13 2.024(9) . ? 
Ni1 N5 2.251(9) . ? 
Ni1 N12 2.255(9) . ? 
Ni1 N6 2.321(8) . ? 
Ni2 O6 2.070(8) . ? 
Ni2 O1 2.073(8) . ? 
Ni2 N7 2.096(9) . ? 
Ni2 O2 2.099(7) . ? 
Ni2 N2 2.108(10) . ? 
Ni2 N10 2.109(8) . ? 
O1 N13 1.335(11) . ? 
B1 F3 1.30(3) . ? 
B1 F3A 1.32(5) . ? 
B1 F1 1.34(3) . ? 
B1 F2 1.358(18) . ? 
B1 F4 1.37(3) . ? 
B1 F4A 1.40(3) . ? 
B1 F1A 1.48(4) . ? 
O2 N16 1.330(11) . ? 
N2 C14 1.471(16) . ? 
N2 C40 1.503(16) . ? 
N2 C4 1.504(15) . ? 
C2 C20 1.386(19) . ? 
C2 C21 1.389(17) . ? 
C2 H2A 0.9300 . ? 
C4 C7 1.49(2) . ? 
C4 H4A 0.9700 . ? 
C4 H4B 0.9700 . ? 
Br5 C47 1.898(13) . ? 
N5 C50 1.337(14) . ? 
N5 C44 1.367(14) . ? 
Br6 C53 1.872(13) . ? 
O6 N17 1.346(10) . ? 
N6 C47 1.325(14) . ? 
N6 C17 1.374(14) . ? 
C6 C26 1.35(2) . ? 
C6 C47 1.388(17) . ? 
C6 H6A 0.9300 . ? 
N7 C7 1.484(16) . ? 
N7 C51 1.495(17) . ? 
N7 C34 1.501(15) . ? 
C7 H7A 0.9531 . ? 
C7 H7B 0.9440 . ? 
N10 C29 1.459(14) . ? 
N10 C27 1.477(15) . ? 
N10 C19 1.510(15) . ? 
C11 C20 1.36(2) . ? 
C11 C53 1.405(18) . ? 
C11 H11A 0.9300 . ? 
N12 C53 1.341(14) . ? 
N12 C21 1.373(15) . ? 
N13 C31 1.279(14) . ? 
C14 H14A 0.9600 . ? 
C14 H14B 0.9600 . ? 
C14 H14C 0.9600 . ? 
C15 C36 1.357(19) . ? 
C15 C44 1.388(17) . ? 
C15 H15A 0.9300 . ? 
N16 C45 1.264(14) . ? 
N17 C41 1.283(14) . ? 
C17 C28 1.386(16) . ? 
C17 C41 1.437(16) . ? 
C19 C34 1.475(19) . ? 
C19 H19A 0.9700 . ? 
C19 H19B 0.9700 . ? 
C20 H20A 0.9300 . ? 
C21 C31 1.455(16) . ? 
C26 C28 1.369(19) . ? 
C26 H26A 0.9300 . ? 
C27 H27A 0.9600 . ? 
C27 H27B 0.9600 . ? 
C27 H27C 0.9600 . ? 
C28 H28A 0.9300 . ? 
C29 C40 1.507(19) . ? 
C29 H29A 0.9700 . ? 
C29 H29B 0.9700 . ? 
C31 H31A 0.9300 . ? 
C34 H34A 0.9700 . ? 
C34 H34B 0.9700 . ? 
C36 C46 1.352(19) . ? 
C36 H36A 0.9300 . ? 
C40 H40A 0.9700 . ? 
C40 H40B 0.9700 . ? 
C41 H41A 0.9300 . ? 
C44 C45 1.476(15) . ? 
C45 H45A 0.9300 . ? 
C46 C50 1.399(17) . ? 
C46 H46A 0.9300 . ? 
C51 H51A 0.9600 . ? 
C51 H51B 0.9600 . ? 
C51 H51C 0.9600 . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N17 Ni1 N16 88.4(3) . . ? 
N17 Ni1 N13 88.9(4) . . ? 
N16 Ni1 N13 90.3(4) . . ? 
N17 Ni1 N5 93.6(3) . . ? 
N16 Ni1 N5 78.1(3) . . ? 
N13 Ni1 N5 168.0(3) . . ? 
N17 Ni1 N12 164.5(3) . . ? 
N16 Ni1 N12 97.1(3) . . ? 
N13 Ni1 N12 76.7(3) . . ? 
N5 Ni1 N12 101.7(3) . . ? 
N17 Ni1 N6 76.3(3) . . ? 
N16 Ni1 N6 164.4(3) . . ? 
N13 Ni1 N6 92.6(3) . . ? 
N5 Ni1 N6 99.4(3) . . ? 
N12 Ni1 N6 98.5(3) . . ? 
O6 Ni2 O1 94.2(3) . . ? 
O6 Ni2 N7 172.3(3) . . ? 
O1 Ni2 N7 93.1(4) . . ? 
O6 Ni2 O2 92.1(3) . . ? 
O1 Ni2 O2 92.5(3) . . ? 
N7 Ni2 O2 90.3(3) . . ? 
O6 Ni2 N2 88.5(3) . . ? 
O1 Ni2 N2 171.6(3) . . ? 
N7 Ni2 N2 84.0(4) . . ? 
O2 Ni2 N2 95.4(4) . . ? 
O6 Ni2 N10 93.9(3) . . ? 
O1 Ni2 N10 87.9(3) . . ? 
N7 Ni2 N10 83.7(4) . . ? 
O2 Ni2 N10 173.9(3) . . ? 
N2 Ni2 N10 83.9(4) . . ? 
N13 O1 Ni2 113.2(6) . . ? 
F3 B1 F3A 130(3) . . ? 
F3 B1 F1 116(2) . . ? 
F3A B1 F1 37(4) . . ? 
F3 B1 F2 109.5(19) . . ? 
F3A B1 F2 120(2) . . ? 
F1 B1 F2 110.4(15) . . ? 
F3 B1 F4 112(2) . . ? 
F3A B1 F4 68(4) . . ? 
F1 B1 F4 105(2) . . ? 
F2 B1 F4 103.8(18) . . ? 
F3 B1 F4A 51(2) . . ? 
F3A B1 F4A 104(3) . . ? 
F1 B1 F4A 125(2) . . ? 
F2 B1 F4A 124.6(19) . . ? 
F4 B1 F4A 60(2) . . ? 
F3 B1 F1A 62(3) . . ? 
F3A B1 F1A 95(4) . . ? 
F1 B1 F1A 62(3) . . ? 
F2 B1 F1A 103(2) . . ? 
F4 B1 F1A 153(2) . . ? 
F4A B1 F1A 106(3) . . ? 
N16 O2 Ni2 110.1(6) . . ? 
C14 N2 C40 110.9(11) . . ? 
C14 N2 C4 111.6(10) . . ? 
C40 N2 C4 109.2(10) . . ? 
C14 N2 Ni2 112.8(7) . . ? 
C40 N2 Ni2 102.5(7) . . ? 
C4 N2 Ni2 109.3(8) . . ? 
C20 C2 C21 119.6(13) . . ? 
C20 C2 H2A 120.2 . . ? 
C21 C2 H2A 120.2 . . ? 
C7 C4 N2 109.8(10) . . ? 
C7 C4 H4A 109.7 . . ? 
N2 C4 H4A 109.7 . . ? 
C7 C4 H4B 109.7 . . ? 
N2 C4 H4B 109.7 . . ? 
H4A C4 H4B 108.2 . . ? 
C50 N5 C44 114.9(9) . . ? 
C50 N5 Ni1 136.6(7) . . ? 
C44 N5 Ni1 108.6(7) . . ? 
N17 O6 Ni2 110.9(6) . . ? 
C47 N6 C17 115.3(9) . . ? 
C47 N6 Ni1 137.1(8) . . ? 
C17 N6 Ni1 107.5(6) . . ? 
C26 C6 C47 118.2(12) . . ? 
C26 C6 H6A 120.9 . . ? 
C47 C6 H6A 120.9 . . ? 
C7 N7 C51 110.3(11) . . ? 
C7 N7 C34 110.2(10) . . ? 
C51 N7 C34 111.1(10) . . ? 
C7 N7 Ni2 103.4(7) . . ? 
C51 N7 Ni2 112.2(7) . . ? 
C34 N7 Ni2 109.5(8) . . ? 
N7 C7 C4 113.0(11) . . ? 
N7 C7 H7A 108.4 . . ? 
C4 C7 H7A 108.9 . . ? 
N7 C7 H7B 105.7 . . ? 
C4 C7 H7B 108.9 . . ? 
H7A C7 H7B 112.0 . . ? 
C29 N10 C27 111.0(10) . . ? 
C29 N10 C19 110.5(9) . . ? 
C27 N10 C19 109.9(10) . . ? 
C29 N10 Ni2 109.9(7) . . ? 
C27 N10 Ni2 111.5(7) . . ? 
C19 N10 Ni2 103.7(7) . . ? 
C20 C11 C53 119.1(12) . . ? 
C20 C11 H11A 120.4 . . ? 
C53 C11 H11A 120.4 . . ? 
C53 N12 C21 117.0(10) . . ? 
C53 N12 Ni1 134.4(8) . . ? 
C21 N12 Ni1 107.4(7) . . ? 
C31 N13 O1 119.1(9) . . ? 
C31 N13 Ni1 118.8(7) . . ? 
O1 N13 Ni1 122.0(7) . . ? 
N2 C14 H14A 109.5 . . ? 
N2 C14 H14B 109.5 . . ? 
H14A C14 H14B 109.5 . . ? 
N2 C14 H14C 109.5 . . ? 
H14A C14 H14C 109.5 . . ? 
H14B C14 H14C 109.5 . . ? 
C36 C15 C44 119.6(13) . . ? 
C36 C15 H15A 120.2 . . ? 
C44 C15 H15A 120.2 . . ? 
C45 N16 O2 119.4(9) . . ? 
C45 N16 Ni1 118.0(8) . . ? 
O2 N16 Ni1 122.2(7) . . ? 
C41 N17 O6 118.6(9) . . ? 
C41 N17 Ni1 119.7(7) . . ? 
O6 N17 Ni1 121.5(6) . . ? 
N6 C17 C28 121.5(11) . . ? 
N6 C17 C41 116.4(9) . . ? 
C28 C17 C41 122.1(11) . . ? 
C34 C19 N10 111.4(10) . . ? 
C34 C19 H19A 109.3 . . ? 
N10 C19 H19A 109.3 . . ? 
C34 C19 H19B 109.3 . . ? 
N10 C19 H19B 109.3 . . ? 
H19A C19 H19B 108.0 . . ? 
C11 C20 C2 119.2(12) . . ? 
C11 C20 H20A 120.4 . . ? 
C2 C20 H20A 120.4 . . ? 
N12 C21 C2 121.9(11) . . ? 
N12 C21 C31 117.0(10) . . ? 
C2 C21 C31 121.1(12) . . ? 
C6 C26 C28 118.7(13) . . ? 
C6 C26 H26A 120.7 . . ? 
C28 C26 H26A 120.7 . . ? 
N10 C27 H27A 109.5 . . ? 
N10 C27 H27B 109.5 . . ? 
H27A C27 H27B 109.5 . . ? 
N10 C27 H27C 109.5 . . ? 
H27A C27 H27C 109.5 . . ? 
H27B C27 H27C 109.5 . . ? 
C26 C28 C17 120.7(14) . . ? 
C26 C28 H28A 119.7 . . ? 
C17 C28 H28A 119.7 . . ? 
N10 C29 C40 111.4(10) . . ? 
N10 C29 H29A 109.3 . . ? 
C40 C29 H29A 109.3 . . ? 
N10 C29 H29B 109.3 . . ? 
C40 C29 H29B 109.3 . . ? 
H29A C29 H29B 108.0 . . ? 
N13 C31 C21 116.9(11) . . ? 
N13 C31 H31A 121.6 . . ? 
C21 C31 H31A 121.6 . . ? 
C19 C34 N7 112.1(10) . . ? 
C19 C34 H34A 109.2 . . ? 
N7 C34 H34A 109.2 . . ? 
C19 C34 H34B 109.2 . . ? 
N7 C34 H34B 109.2 . . ? 
H34A C34 H34B 107.9 . . ? 
C46 C36 C15 120.2(12) . . ? 
C46 C36 H36A 119.9 . . ? 
C15 C36 H36A 119.9 . . ? 
N2 C40 C29 111.9(11) . . ? 
N2 C40 H40A 109.2 . . ? 
C29 C40 H40A 109.2 . . ? 
N2 C40 H40B 109.2 . . ? 
C29 C40 H40B 109.2 . . ? 
H40A C40 H40B 107.9 . . ? 
N17 C41 C17 119.7(10) . . ? 
N17 C41 H41A 120.1 . . ? 
C17 C41 H41A 120.1 . . ? 
N5 C44 C15 122.7(11) . . ? 
N5 C44 C45 115.8(10) . . ? 
C15 C44 C45 121.5(11) . . ? 
N16 C45 C44 119.6(10) . . ? 
N16 C45 H45A 120.2 . . ? 
C44 C45 H45A 120.2 . . ? 
C36 C46 C50 117.4(12) . . ? 
C36 C46 H46A 121.3 . . ? 
C50 C46 H46A 121.3 . . ? 
N6 C47 C6 125.7(12) . . ? 
N6 C47 Br5 118.2(9) . . ? 
C6 C47 Br5 116.1(9) . . ? 
N5 C50 C46 125.2(11) . . ? 
N5 C50 Br1 117.5(8) . . ? 
C46 C50 Br1 117.3(9) . . ? 
N7 C51 H51A 109.5 . . ? 
N7 C51 H51B 109.5 . . ? 
H51A C51 H51B 109.5 . . ? 
N7 C51 H51C 109.5 . . ? 
H51A C51 H51C 109.5 . . ? 
H51B C51 H51C 109.5 . . ? 
N12 C53 C11 123.1(12) . . ? 
N12 C53 Br6 119.6(9) . . ? 
C11 C53 Br6 117.2(9) . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O6 Ni2 O1 N13 -69.7(7) . . . . ? 
N7 Ni2 O1 N13 112.9(7) . . . . ? 
O2 Ni2 O1 N13 22.5(7) . . . . ? 
N2 Ni2 O1 N13 -178(2) . . . . ? 
N10 Ni2 O1 N13 -163.5(7) . . . . ? 
O6 Ni2 O2 N16 20.1(7) . . . . ? 
O1 Ni2 O2 N16 -74.1(7) . . . . ? 
N7 Ni2 O2 N16 -167.3(7) . . . . ? 
N2 Ni2 O2 N16 108.8(7) . . . . ? 
N10 Ni2 O2 N16 -168(3) . . . . ? 
O6 Ni2 N2 C14 53.2(9) . . . . ? 
O1 Ni2 N2 C14 162(2) . . . . ? 
N7 Ni2 N2 C14 -128.4(9) . . . . ? 
O2 Ni2 N2 C14 -38.7(9) . . . . ? 
N10 Ni2 N2 C14 147.4(9) . . . . ? 
O6 Ni2 N2 C40 -66.1(7) . . . . ? 
O1 Ni2 N2 C40 42(3) . . . . ? 
N7 Ni2 N2 C40 112.2(8) . . . . ? 
O2 Ni2 N2 C40 -158.1(7) . . . . ? 
N10 Ni2 N2 C40 28.0(7) . . . . ? 
O6 Ni2 N2 C4 178.0(8) . . . . ? 
O1 Ni2 N2 C4 -74(3) . . . . ? 
N7 Ni2 N2 C4 -3.6(8) . . . . ? 
O2 Ni2 N2 C4 86.1(8) . . . . ? 
N10 Ni2 N2 C4 -87.8(8) . . . . ? 
C14 N2 C4 C7 104.4(13) . . . . ? 
C40 N2 C4 C7 -132.6(11) . . . . ? 
Ni2 N2 C4 C7 -21.1(13) . . . . ? 
N17 Ni1 N5 C50 91.5(11) . . . . ? 
N16 Ni1 N5 C50 179.1(11) . . . . ? 
N13 Ni1 N5 C50 -166.7(15) . . . . ? 
N12 Ni1 N5 C50 -86.0(11) . . . . ? 
N6 Ni1 N5 C50 14.8(11) . . . . ? 
N17 Ni1 N5 C44 -87.1(7) . . . . ? 
N16 Ni1 N5 C44 0.5(7) . . . . ? 
N13 Ni1 N5 C44 15(2) . . . . ? 
N12 Ni1 N5 C44 95.4(7) . . . . ? 
N6 Ni1 N5 C44 -163.8(7) . . . . ? 
O1 Ni2 O6 N17 18.2(6) . . . . ? 
N7 Ni2 O6 N17 178(85) . . . . ? 
O2 Ni2 O6 N17 -74.5(6) . . . . ? 
N2 Ni2 O6 N17 -169.8(6) . . . . ? 
N10 Ni2 O6 N17 106.4(6) . . . . ? 
N17 Ni1 N6 C47 179.8(11) . . . . ? 
N16 Ni1 N6 C47 -168.2(12) . . . . ? 
N13 Ni1 N6 C47 91.6(11) . . . . ? 
N5 Ni1 N6 C47 -88.7(11) . . . . ? 
N12 Ni1 N6 C47 14.7(11) . . . . ? 
N17 Ni1 N6 C17 -4.7(7) . . . . ? 
N16 Ni1 N6 C17 7.3(16) . . . . ? 
N13 Ni1 N6 C17 -93.0(7) . . . . ? 
N5 Ni1 N6 C17 86.7(7) . . . . ? 
N12 Ni1 N6 C17 -169.8(7) . . . . ? 
O6 Ni2 N7 C7 39(3) . . . . ? 
O1 Ni2 N7 C7 -161.2(7) . . . . ? 
O2 Ni2 N7 C7 -68.7(7) . . . . ? 
N2 Ni2 N7 C7 26.7(7) . . . . ? 
N10 Ni2 N7 C7 111.2(8) . . . . ? 
O6 Ni2 N7 C51 158(2) . . . . ? 
O1 Ni2 N7 C51 -42.4(9) . . . . ? 
O2 Ni2 N7 C51 50.2(9) . . . . ? 
N2 Ni2 N7 C51 145.6(9) . . . . ? 
N10 Ni2 N7 C51 -129.9(9) . . . . ? 
O6 Ni2 N7 C34 -78(3) . . . . ? 
O1 Ni2 N7 C34 81.4(8) . . . . ? 
O2 Ni2 N7 C34 173.9(8) . . . . ? 
N2 Ni2 N7 C34 -90.7(9) . . . . ? 
N10 Ni2 N7 C34 -6.2(8) . . . . ? 
C51 N7 C7 C4 -168.1(11) . . . . ? 
C34 N7 C7 C4 68.9(13) . . . . ? 
Ni2 N7 C7 C4 -48.0(11) . . . . ? 
N2 C4 C7 N7 47.7(15) . . . . ? 
O6 Ni2 N10 C29 82.4(8) . . . . ? 
O1 Ni2 N10 C29 176.5(8) . . . . ? 
N7 Ni2 N10 C29 -90.2(8) . . . . ? 
O2 Ni2 N10 C29 -89(3) . . . . ? 
N2 Ni2 N10 C29 -5.6(8) . . . . ? 
O6 Ni2 N10 C27 -41.2(8) . . . . ? 
O1 Ni2 N10 C27 52.9(8) . . . . ? 
N7 Ni2 N10 C27 146.2(9) . . . . ? 
O2 Ni2 N10 C27 147(3) . . . . ? 
N2 Ni2 N10 C27 -129.2(8) . . . . ? 
O6 Ni2 N10 C19 -159.4(7) . . . . ? 
O1 Ni2 N10 C19 -65.4(7) . . . . ? 
N7 Ni2 N10 C19 28.0(7) . . . . ? 
O2 Ni2 N10 C19 29(3) . . . . ? 
N2 Ni2 N10 C19 112.6(7) . . . . ? 
N17 Ni1 N12 C53 -160.1(12) . . . . ? 
N16 Ni1 N12 C53 89.9(11) . . . . ? 
N13 Ni1 N12 C53 178.5(11) . . . . ? 
N5 Ni1 N12 C53 10.6(11) . . . . ? 
N6 Ni1 N12 C53 -90.9(11) . . . . ? 
N17 Ni1 N12 C21 6.5(16) . . . . ? 
N16 Ni1 N12 C21 -103.5(7) . . . . ? 
N13 Ni1 N12 C21 -14.9(7) . . . . ? 
N5 Ni1 N12 C21 177.2(7) . . . . ? 
N6 Ni1 N12 C21 75.7(7) . . . . ? 
Ni2 O1 N13 C31 -139.0(9) . . . . ? 
Ni2 O1 N13 Ni1 45.5(9) . . . . ? 
N17 Ni1 N13 C31 -158.9(9) . . . . ? 
N16 Ni1 N13 C31 112.7(9) . . . . ? 
N5 Ni1 N13 C31 98.8(18) . . . . ? 
N12 Ni1 N13 C31 15.5(9) . . . . ? 
N6 Ni1 N13 C31 -82.6(9) . . . . ? 
N17 Ni1 N13 O1 16.6(8) . . . . ? 
N16 Ni1 N13 O1 -71.7(8) . . . . ? 
N5 Ni1 N13 O1 -85.7(18) . . . . ? 
N12 Ni1 N13 O1 -169.0(8) . . . . ? 
N6 Ni1 N13 O1 92.9(7) . . . . ? 
Ni2 O2 N16 C45 -120.3(9) . . . . ? 
Ni2 O2 N16 Ni1 51.5(8) . . . . ? 
N17 Ni1 N16 C45 94.3(9) . . . . ? 
N13 Ni1 N16 C45 -176.9(9) . . . . ? 
N5 Ni1 N16 C45 0.2(9) . . . . ? 
N12 Ni1 N16 C45 -100.3(9) . . . . ? 
N6 Ni1 N16 C45 82.5(15) . . . . ? 
N17 Ni1 N16 O2 -77.6(8) . . . . ? 
N13 Ni1 N16 O2 11.3(8) . . . . ? 
N5 Ni1 N16 O2 -171.7(8) . . . . ? 
N12 Ni1 N16 O2 87.9(8) . . . . ? 
N6 Ni1 N16 O2 -89.3(15) . . . . ? 
Ni2 O6 N17 C41 -123.4(9) . . . . ? 
Ni2 O6 N17 Ni1 51.8(8) . . . . ? 
N16 Ni1 N17 C41 -172.3(9) . . . . ? 
N13 Ni1 N17 C41 97.4(9) . . . . ? 
N5 Ni1 N17 C41 -94.3(9) . . . . ? 
N12 Ni1 N17 C41 76.6(15) . . . . ? 
N6 Ni1 N17 C41 4.5(8) . . . . ? 
N16 Ni1 N17 O6 12.5(7) . . . . ? 
N13 Ni1 N17 O6 -77.8(7) . . . . ? 
N5 Ni1 N17 O6 90.5(7) . . . . ? 
N12 Ni1 N17 O6 -98.6(14) . . . . ? 
N6 Ni1 N17 O6 -170.7(8) . . . . ? 
C47 N6 C17 C28 0.4(16) . . . . ? 
Ni1 N6 C17 C28 -176.2(10) . . . . ? 
C47 N6 C17 C41 -178.7(10) . . . . ? 
Ni1 N6 C17 C41 4.7(11) . . . . ? 
C29 N10 C19 C34 70.7(13) . . . . ? 
C27 N10 C19 C34 -166.4(10) . . . . ? 
Ni2 N10 C19 C34 -47.0(11) . . . . ? 
C53 C11 C20 C2 0(2) . . . . ? 
C21 C2 C20 C11 -1(2) . . . . ? 
C53 N12 C21 C2 3.2(16) . . . . ? 
Ni1 N12 C21 C2 -166.1(10) . . . . ? 
C53 N12 C21 C31 -177.0(10) . . . . ? 
Ni1 N12 C21 C31 13.7(12) . . . . ? 
C20 C2 C21 N12 -0.4(19) . . . . ? 
C20 C2 C21 C31 179.9(12) . . . . ? 
C47 C6 C26 C28 0(2) . . . . ? 
C6 C26 C28 C17 1(2) . . . . ? 
N6 C17 C28 C26 -1(2) . . . . ? 
C41 C17 C28 C26 178.0(13) . . . . ? 
C27 N10 C29 C40 104.6(12) . . . . ? 
C19 N10 C29 C40 -133.1(11) . . . . ? 
Ni2 N10 C29 C40 -19.2(13) . . . . ? 
O1 N13 C31 C21 171.4(9) . . . . ? 
Ni1 N13 C31 C21 -12.9(14) . . . . ? 
N12 C21 C31 N13 -2.3(16) . . . . ? 
C2 C21 C31 N13 177.4(11) . . . . ? 
N10 C19 C34 N7 45.2(15) . . . . ? 
C7 N7 C34 C19 -131.7(12) . . . . ? 
C51 N7 C34 C19 105.8(13) . . . . ? 
Ni2 N7 C34 C19 -18.7(14) . . . . ? 
C44 C15 C36 C46 -2(2) . . . . ? 
C14 N2 C40 C29 -168.1(10) . . . . ? 
C4 N2 C40 C29 68.4(13) . . . . ? 
Ni2 N2 C40 C29 -47.4(11) . . . . ? 
N10 C29 C40 N2 46.5(15) . . . . ? 
O6 N17 C41 C17 171.9(9) . . . . ? 
Ni1 N17 C41 C17 -3.4(14) . . . . ? 
N6 C17 C41 N17 -1.5(16) . . . . ? 
C28 C17 C41 N17 179.3(11) . . . . ? 
C50 N5 C44 C15 -0.5(17) . . . . ? 
Ni1 N5 C44 C15 178.5(11) . . . . ? 
C50 N5 C44 C45 -179.9(10) . . . . ? 
Ni1 N5 C44 C45 -1.0(12) . . . . ? 
C36 C15 C44 N5 1(2) . . . . ? 
C36 C15 C44 C45 -179.7(13) . . . . ? 
O2 N16 C45 C44 171.3(9) . . . . ? 
Ni1 N16 C45 C44 -0.8(15) . . . . ? 
N5 C44 C45 N16 1.3(16) . . . . ? 
C15 C44 C45 N16 -178.2(12) . . . . ? 
C15 C36 C46 C50 3(2) . . . . ? 
C17 N6 C47 C6 0.3(17) . . . . ? 
Ni1 N6 C47 C6 175.5(9) . . . . ? 
C17 N6 C47 Br5 -178.2(7) . . . . ? 
Ni1 N6 C47 Br5 -3.0(15) . . . . ? 
C26 C6 C47 N6 0(2) . . . . ? 
C26 C6 C47 Br5 178.2(11) . . . . ? 
C44 N5 C50 C46 1.3(17) . . . . ? 
Ni1 N5 C50 C46 -177.3(9) . . . . ? 
C44 N5 C50 Br1 -177.7(8) . . . . ? 
Ni1 N5 C50 Br1 3.8(15) . . . . ? 
C36 C46 C50 N5 -2(2) . . . . ? 
C36 C46 C50 Br1 176.5(11) . . . . ? 
C21 N12 C53 C11 -4.5(16) . . . . ? 
Ni1 N12 C53 C11 161.1(9) . . . . ? 
C21 N12 C53 Br6 173.8(8) . . . . ? 
Ni1 N12 C53 Br6 -20.6(15) . . . . ? 
C20 C11 C53 N12 2.9(19) . . . . ? 
C20 C11 C53 Br6 -175.4(10) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.996 
_diffrn_reflns_theta_full              24.99 
_diffrn_measured_fraction_theta_full   0.996 
_refine_diff_density_max    1.037 
_refine_diff_density_min   -0.715 
_refine_diff_density_rms    0.179 

#===End

data_3 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C54 H71 B N12 Ni2 O6' 
_chemical_formula_weight          1112.46 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'B'  'B'   0.0013   0.0007 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ni'  'Ni'   0.3393   1.1124 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/c 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y-1/2, z-1/2' 
  
_cell_length_a                    9.1157(18) 
_cell_length_b                    30.055(6) 
_cell_length_c                    21.282(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  93.25(3) 
_cell_angle_gamma                 90.00 
_cell_volume                      5821(2) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     293(2) 
_cell_measurement_reflns_used     35468 
_cell_measurement_theta_min       3.03 
_cell_measurement_theta_max       27.5 
  
_exptl_crystal_description        block 
_exptl_crystal_colour             'red brown' 
_exptl_crystal_size_max           0.19 
_exptl_crystal_size_mid           0.16 
_exptl_crystal_size_min           0.12 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.269 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              2352 
_exptl_absorpt_coefficient_mu     0.704 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.392 
_exptl_absorpt_correction_T_max   1.000 
_exptl_absorpt_process_details    'ABSCOR; T Higashi (2001)' 
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   graphite 
_diffrn_measurement_device_type   'Rigaku R-AXIS RAPID IP' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  0.77 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             51836 
_diffrn_reflns_av_R_equivalents   0.0564 
_diffrn_reflns_av_sigmaI/netI     0.0513 
_diffrn_reflns_limit_h_min        -11 
_diffrn_reflns_limit_h_max        11 
_diffrn_reflns_limit_k_min        -38 
_diffrn_reflns_limit_k_max        38 
_diffrn_reflns_limit_l_min        -26 
_diffrn_reflns_limit_l_max        27 
_diffrn_reflns_theta_min          3.02 
_diffrn_reflns_theta_max          27.46 
_reflns_number_total              13137 
_reflns_number_gt                 8927 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_cell_refinement        'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_reduction         'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'XP (Sheldrick, 1998)' 
_computing_publication_material   'XP (Sheldrick, 1998)' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
  
_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.0988P)²+1.3768P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          13137 
_refine_ls_number_parameters      676 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0862 
_refine_ls_R_factor_gt            0.0561 
_refine_ls_wR_factor_ref          0.1804 
_refine_ls_wR_factor_gt           0.1593 
_refine_ls_goodness_of_fit_ref    1.051 
_refine_ls_restrained_S_all       1.051 
_refine_ls_shift/su_max           0.002 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ni1 Ni 0.50258(4) 0.552715(12) 0.266888(17) 0.04092(12) Uani 1 1 d . . . 
Ni2 Ni 0.40699(5) 0.440464(12) 0.250013(18) 0.04723(13) Uani 1 1 d . . . 
O3 O 0.5806(3) 0.46690(7) 0.20208(10) 0.0544(5) Uani 1 1 d . . . 
O2 O 0.4703(2) 0.46727(6) 0.33846(10) 0.0499(5) Uani 1 1 d . . . 
O1 O 0.2554(2) 0.48998(7) 0.22339(10) 0.0522(5) Uani 1 1 d . . . 
N12 N 0.4015(3) 0.59763(8) 0.32856(12) 0.0445(5) Uani 1 1 d . . . 
N11 N 0.4523(3) 0.51277(8) 0.33856(11) 0.0435(5) Uani 1 1 d . . . 
N10 N 0.6322(3) 0.50540(8) 0.23046(12) 0.0465(6) Uani 1 1 d . . . 
N9 N 0.7178(3) 0.57518(8) 0.29552(12) 0.0461(6) Uani 1 1 d . . . 
N8 N 0.2375(3) 0.40248(9) 0.29147(14) 0.0599(7) Uani 1 1 d . . . 
C50 C 0.5498(3) 0.75528(10) -0.01250(16) 0.0502(7) Uani 1 1 d . . . 
N7 N 0.4905(3) 0.59808(8) 0.19083(12) 0.0482(6) Uani 1 1 d . . . 
N6 N 0.3259(3) 0.52957(8) 0.21402(12) 0.0454(6) Uani 1 1 d . . . 
C49 C 0.2834(3) 0.55220(10) 0.16471(15) 0.0491(7) Uani 1 1 d . . . 
C48 C 0.7701(3) 0.75517(10) -0.09543(15) 0.0520(7) Uani 1 1 d . . . 
N5 N 0.3520(4) 0.50563(10) 0.43741(14) 0.0661(8) Uani 1 1 d . . . 
H5A H 0.3634 0.4772 0.4381 0.079 Uiso 1 1 calc R . . 
H5B H 0.3139 0.5188 0.4684 0.079 Uiso 1 1 calc R . . 
C47 C 0.8236(3) 0.55190(11) 0.26749(15) 0.0507(7) Uani 1 1 d . . . 
N4 N 0.3372(4) 0.40175(10) 0.16782(14) 0.0653(8) Uani 1 1 d . . . 
C46 C 0.7728(3) 0.51177(11) 0.23419(15) 0.0508(7) Uani 1 1 d . . . 
C45 C 0.3704(3) 0.59198(11) 0.15173(15) 0.0510(7) Uani 1 1 d . . . 
C44 C 0.3944(3) 0.52982(10) 0.38700(14) 0.0463(7) Uani 1 1 d . . . 
C43 C 0.3755(3) 0.64107(10) 0.32150(17) 0.0535(8) Uani 1 1 d . . . 
H43A H 0.4000 0.6546 0.2842 0.064 Uiso 1 1 calc R . . 
C42 C 0.3666(3) 0.57843(10) 0.38347(14) 0.0461(7) Uani 1 1 d . . . 
C41 C 0.5803(4) 0.63201(11) 0.17863(17) 0.0585(8) Uani 1 1 d . . . 
H41A H 0.6632 0.6364 0.2054 0.070 Uiso 1 1 calc R . . 
N3 N 0.5344(3) 0.38055(9) 0.27148(14) 0.0612(7) Uani 1 1 d . . . 
B1 B 0.7271(4) 0.76244(12) -0.02177(18) 0.0487(8) Uani 1 1 d . . . 
C40 C 0.7566(4) 0.61155(11) 0.32849(15) 0.0530(8) Uani 1 1 d . . . 
H40A H 0.6841 0.6274 0.3479 0.064 Uiso 1 1 calc R . . 
C39 C 0.8102(3) 0.72558(11) 0.02477(16) 0.0516(7) Uani 1 1 d . . . 
C38 C 0.3048(4) 0.60252(12) 0.43067(17) 0.0590(8) Uani 1 1 d . . . 
H38A H 0.2808 0.5886 0.4678 0.071 Uiso 1 1 calc R . . 
C37 C 0.7753(3) 0.81453(11) -0.00623(15) 0.0511(7) Uani 1 1 d . . . 
N2 N 0.8713(3) 0.48266(12) 0.20941(17) 0.0752(9) Uani 1 1 d . . . 
H2A H 0.8401 0.4590 0.1904 0.090 Uiso 1 1 calc R . . 
H2B H 0.9640 0.4882 0.2130 0.090 Uiso 1 1 calc R . . 
C36 C 0.4553(4) 0.73110(11) -0.05342(18) 0.0567(8) Uani 1 1 d . . . 
H36A H 0.4924 0.7188 -0.0894 0.068 Uiso 1 1 calc R . . 
C35 C 0.4856(4) 0.77174(13) 0.04111(19) 0.0658(9) Uani 1 1 d . . . 
H35A H 0.5437 0.7877 0.0705 0.079 Uiso 1 1 calc R . . 
C34 C 0.9202(4) 0.82722(13) 0.01106(19) 0.0661(9) Uani 1 1 d . . . 
H34A H 0.9911 0.8052 0.0178 0.079 Uiso 1 1 calc R . . 
C33 C 0.9613(5) 0.87142(14) 0.0185(2) 0.0742(11) Uani 1 1 d . . . 
H33A H 1.0580 0.8784 0.0308 0.089 Uiso 1 1 calc R . . 
C32 C 0.8995(4) 0.62658(15) 0.3350(2) 0.0749(11) Uani 1 1 d . . . 
H32A H 0.9232 0.6520 0.3583 0.090 Uiso 1 1 calc R . . 
C31 C 0.9050(4) 0.73707(14) -0.11092(19) 0.0698(10) Uani 1 1 d . . . 
H31A H 0.9702 0.7274 -0.0786 0.084 Uiso 1 1 calc R . . 
C30 C 0.6774(4) 0.84965(11) -0.01639(16) 0.0595(8) Uani 1 1 d . . . 
H30A H 0.5800 0.8431 -0.0282 0.071 Uiso 1 1 calc R . . 
C29 C 0.3139(4) 0.66715(11) 0.36674(19) 0.0607(9) Uani 1 1 d . . . 
H29A H 0.2966 0.6973 0.3597 0.073 Uiso 1 1 calc R . . 
C28 C 0.2490(4) 0.74183(14) 0.0095(2) 0.0738(11) Uani 1 1 d . . . 
H28A H 0.1500 0.7379 0.0163 0.089 Uiso 1 1 calc R . . 
N1 N 0.1649(3) 0.54011(11) 0.12468(15) 0.0680(8) Uani 1 1 d . . . 
H1A H 0.1156 0.5165 0.1321 0.082 Uiso 1 1 calc R . . 
H1B H 0.1407 0.5562 0.0924 0.082 Uiso 1 1 calc R . . 
C27 C 0.3074(4) 0.72457(13) -0.0426(2) 0.0668(10) Uani 1 1 d . . . 
H27A H 0.2483 0.7083 -0.0713 0.080 Uiso 1 1 calc R . . 
C26 C 0.2792(4) 0.64768(12) 0.42192(19) 0.0654(9) Uani 1 1 d . . . 
H26A H 0.2389 0.6645 0.4533 0.079 Uiso 1 1 calc R . . 
C25 C 0.3387(5) 0.62002(14) 0.1012(2) 0.0753(11) Uani 1 1 d . . . 
H25A H 0.2539 0.6159 0.0755 0.090 Uiso 1 1 calc R . . 
C24 C 0.3196(5) 0.37258(15) 0.3364(2) 0.0861(13) Uani 1 1 d . . . 
H24A H 0.3539 0.3897 0.3729 0.103 Uiso 1 1 calc R . . 
H24B H 0.2532 0.3499 0.3504 0.103 Uiso 1 1 calc R . . 
C23 C 0.8718(4) 0.73426(14) 0.08494(17) 0.0662(9) Uani 1 1 d . . . 
H23A H 0.8694 0.7632 0.1002 0.079 Uiso 1 1 calc R . . 
C22 C 0.8616(5) 0.90468(13) 0.00804(19) 0.0727(11) Uani 1 1 d . . . 
H22A H 0.8902 0.9342 0.0129 0.087 Uiso 1 1 calc R . . 
C21 C 0.8156(4) 0.68075(12) 0.00682(19) 0.0668(9) Uani 1 1 d . . . 
H21A H 0.7747 0.6729 -0.0327 0.080 Uiso 1 1 calc R . . 
C20 C 0.8512(7) 0.74698(16) -0.2221(2) 0.0959(16) Uani 1 1 d . . . 
H20A H 0.8774 0.7440 -0.2635 0.115 Uiso 1 1 calc R . . 
C19 C 0.7186(5) 0.89432(12) -0.00974(18) 0.0682(10) Uani 1 1 d . . . 
H19A H 0.6497 0.9168 -0.0173 0.082 Uiso 1 1 calc R . . 
C18 C 0.3380(4) 0.76510(15) 0.0520(2) 0.0764(11) Uani 1 1 d . . . 
H18A H 0.2997 0.7765 0.0883 0.092 Uiso 1 1 calc R . . 
C17 C 0.8782(5) 0.64766(15) 0.0444(2) 0.0826(12) Uani 1 1 d . . . 
H17A H 0.8782 0.6184 0.0301 0.099 Uiso 1 1 calc R . . 
C16 C 0.7168(6) 0.76560(15) -0.2086(2) 0.0857(13) Uani 1 1 d . . . 
H16A H 0.6519 0.7753 -0.2411 0.103 Uiso 1 1 calc R . . 
C15 C 0.6804(5) 0.76966(12) -0.14692(18) 0.0690(10) Uani 1 1 d . . . 
H15A H 0.5909 0.7828 -0.1390 0.083 Uiso 1 1 calc R . . 
C14 C 0.9689(4) 0.56516(16) 0.2733(2) 0.0778(12) Uani 1 1 d . . . 
H14A H 1.0411 0.5485 0.2550 0.093 Uiso 1 1 calc R . . 
C13 C 0.9404(5) 0.65783(17) 0.1029(2) 0.0870(13) Uani 1 1 d . . . 
H13A H 0.9840 0.6358 0.1284 0.104 Uiso 1 1 calc R . . 
C12 C 0.5563(5) 0.66072(13) 0.1285(2) 0.0739(11) Uani 1 1 d . . . 
H12A H 0.6212 0.6838 0.1214 0.089 Uiso 1 1 calc R . . 
C11 C 0.4450(5) 0.35096(15) 0.3098(2) 0.0904(14) Uani 1 1 d . . . 
H11A H 0.4097 0.3263 0.2838 0.108 Uiso 1 1 calc R . . 
H11B H 0.5077 0.3388 0.3440 0.108 Uiso 1 1 calc R . . 
C10 C 0.1768(6) 0.39308(18) 0.1793(2) 0.0974(15) Uani 1 1 d . . . 
H10A H 0.1215 0.4202 0.1708 0.117 Uiso 1 1 calc R . . 
H10B H 0.1394 0.3707 0.1497 0.117 Uiso 1 1 calc R . . 
C9 C 0.6809(5) 0.38972(14) 0.3027(2) 0.0790(11) Uani 1 1 d . . . 
H9A H 0.7318 0.3622 0.3108 0.119 Uiso 1 1 calc R . . 
H9B H 0.6690 0.4049 0.3418 0.119 Uiso 1 1 calc R . . 
H9C H 0.7367 0.4080 0.2759 0.119 Uiso 1 1 calc R . . 
C8 C 0.1388(4) 0.43090(14) 0.32698(18) 0.0694(10) Uani 1 1 d . . . 
H8A H 0.0649 0.4128 0.3447 0.104 Uiso 1 1 calc R . . 
H8B H 0.0927 0.4525 0.2991 0.104 Uiso 1 1 calc R . . 
H8C H 0.1948 0.4459 0.3602 0.104 Uiso 1 1 calc R . . 
C7 C 0.5531(5) 0.36149(15) 0.2082(2) 0.0858(13) Uani 1 1 d . . . 
H7A H 0.6268 0.3788 0.1879 0.103 Uiso 1 1 calc R . . 
H7B H 0.5905 0.3314 0.2133 0.103 Uiso 1 1 calc R . . 
C6 C 0.4341(5) 0.65411(15) 0.0896(2) 0.0843(13) Uani 1 1 d . . . 
H6A H 0.4153 0.6727 0.0551 0.101 Uiso 1 1 calc R . . 
C5 C 0.1516(5) 0.37860(15) 0.2414(2) 0.0825(12) Uani 1 1 d . . . 
H5C H 0.1746 0.3471 0.2447 0.099 Uiso 1 1 calc R . . 
H5D H 0.0480 0.3821 0.2484 0.099 Uiso 1 1 calc R . . 
C4 C 0.9369(5) 0.70121(18) 0.1232(2) 0.0859(13) Uani 1 1 d . . . 
H4A H 0.9784 0.7086 0.1627 0.103 Uiso 1 1 calc R . . 
C3 C 0.9451(6) 0.73302(17) -0.1726(2) 0.0917(14) Uani 1 1 d . . . 
H3A H 1.0359 0.7208 -0.1808 0.110 Uiso 1 1 calc R . . 
C2 C 0.4195(7) 0.36011(16) 0.1662(2) 0.1012(17) Uani 1 1 d . . . 
H2C H 0.4464 0.3545 0.1235 0.121 Uiso 1 1 calc R . . 
H2D H 0.3575 0.3358 0.1787 0.121 Uiso 1 1 calc R . . 
C1 C 1.0059(4) 0.60312(18) 0.3062(2) 0.0922(15) Uani 1 1 d . . . 
H1C H 1.1028 0.6129 0.3091 0.111 Uiso 1 1 calc R . . 
O1W O 0.3080(3) 0.96132(11) 0.06843(12) 0.0818(8) Uani 1 1 d . . . 
C51 C 0.3443(5) 0.42636(14) 0.10818(17) 0.0766(11) Uani 1 1 d . . . 
H51A H 0.3123 0.4074 0.0738 0.115 Uiso 1 1 calc R . . 
H51B H 0.4437 0.4357 0.1030 0.115 Uiso 1 1 calc R . . 
H51C H 0.2817 0.4520 0.1089 0.115 Uiso 1 1 calc R . . 
C52 C 0.1840(6) 0.98363(19) 0.0894(2) 0.0924(14) Uani 1 1 d . . . 
O2W O 0.6445(6) 0.48905(17) 0.08039(19) 0.1429(16) Uani 1 1 d . . . 
O3W O 0.8420(8) 0.4372(2) 0.0222(3) 0.195(3) Uani 1 1 d . . . 
C53 C 0.6547(14) 0.5333(3) 0.0671(4) 0.200(5) Uani 1 1 d . . . 
C54 C 0.8343(12) 0.3950(4) 0.0637(5) 0.200(4) Uani 1 1 d . . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Ni1 N11 2.014(2) . ? 
Ni1 N10 2.030(2) . ? 
Ni1 N6 2.034(3) . ? 
Ni1 N7 2.115(2) . ? 
Ni1 N12 2.128(2) . ? 
Ni1 N9 2.131(2) . ? 
Ni2 O3 2.087(2) . ? 
Ni2 O1 2.087(2) . ? 
Ni2 O2 2.098(2) . ? 
Ni2 N8 2.150(3) . ? 
Ni2 N4 2.166(3) . ? 
Ni2 N3 2.177(3) . ? 
O3 N10 1.376(3) . ? 
O2 N11 1.377(3) . ? 
O1 N6 1.372(3) . ? 
N12 C43 1.334(4) . ? 
N12 C42 1.357(4) . ? 
N11 C44 1.290(4) . ? 
N10 C46 1.294(4) . ? 
N9 C40 1.336(4) . ? 
N9 C47 1.357(4) . ? 
N8 C5 1.472(5) . ? 
N8 C8 1.479(5) . ? 
N8 C24 1.483(5) . ? 
C50 C36 1.394(5) . ? 
C50 C35 1.402(5) . ? 
C50 B1 1.654(5) . ? 
N7 C41 1.342(4) . ? 
N7 C45 1.350(4) . ? 
N6 C49 1.291(4) . ? 
C49 N1 1.385(4) . ? 
C49 C45 1.469(4) . ? 
C48 C15 1.399(5) . ? 
C48 C31 1.401(5) . ? 
C48 B1 1.652(5) . ? 
N5 C44 1.369(4) . ? 
N5 H5A 0.8600 . ? 
N5 H5B 0.8600 . ? 
C47 C14 1.383(5) . ? 
C47 C46 1.461(5) . ? 
N4 C2 1.461(5) . ? 
N4 C51 1.474(5) . ? 
N4 C10 1.518(6) . ? 
C46 N2 1.380(4) . ? 
C45 C25 1.383(5) . ? 
C44 C42 1.484(4) . ? 
C43 C29 1.385(5) . ? 
C43 H43A 0.9300 . ? 
C42 C38 1.384(4) . ? 
C41 C12 1.380(5) . ? 
C41 H41A 0.9300 . ? 
N3 C7 1.483(5) . ? 
N3 C11 1.482(5) . ? 
N3 C9 1.483(5) . ? 
B1 C39 1.642(5) . ? 
B1 C37 1.654(5) . ? 
C40 C32 1.379(5) . ? 
C40 H40A 0.9300 . ? 
C39 C23 1.393(5) . ? 
C39 C21 1.402(5) . ? 
C38 C26 1.388(5) . ? 
C38 H38A 0.9300 . ? 
C37 C30 1.391(5) . ? 
C37 C34 1.404(5) . ? 
N2 H2A 0.8600 . ? 
N2 H2B 0.8600 . ? 
C36 C27 1.394(5) . ? 
C36 H36A 0.9300 . ? 
C35 C18 1.392(5) . ? 
C35 H35A 0.9300 . ? 
C34 C33 1.387(5) . ? 
C34 H34A 0.9300 . ? 
C33 C22 1.361(6) . ? 
C33 H33A 0.9300 . ? 
C32 C1 1.370(6) . ? 
C32 H32A 0.9300 . ? 
C31 C3 1.389(6) . ? 
C31 H31A 0.9300 . ? 
C30 C19 1.399(5) . ? 
C30 H30A 0.9300 . ? 
C29 C26 1.365(5) . ? 
C29 H29A 0.9300 . ? 
C28 C27 1.361(6) . ? 
C28 C18 1.372(6) . ? 
C28 H28A 0.9300 . ? 
N1 H1A 0.8600 . ? 
N1 H1B 0.8600 . ? 
C27 H27A 0.9300 . ? 
C26 H26A 0.9300 . ? 
C25 C6 1.376(6) . ? 
C25 H25A 0.9300 . ? 
C24 C11 1.457(6) . ? 
C24 H24A 0.9700 . ? 
C24 H24B 0.9700 . ? 
C23 C4 1.396(6) . ? 
C23 H23A 0.9300 . ? 
C22 C19 1.372(6) . ? 
C22 H22A 0.9300 . ? 
C21 C17 1.379(6) . ? 
C21 H21A 0.9300 . ? 
C20 C3 1.384(7) . ? 
C20 C16 1.392(7) . ? 
C20 H20A 0.9300 . ? 
C19 H19A 0.9300 . ? 
C18 H18A 0.9300 . ? 
C17 C13 1.374(6) . ? 
C17 H17A 0.9300 . ? 
C16 C15 1.378(6) . ? 
C16 H16A 0.9300 . ? 
C15 H15A 0.9300 . ? 
C14 C1 1.371(6) . ? 
C14 H14A 0.9300 . ? 
C13 C4 1.374(7) . ? 
C13 H13A 0.9300 . ? 
C12 C6 1.364(6) . ? 
C12 H12A 0.9300 . ? 
C11 H11A 0.9700 . ? 
C11 H11B 0.9700 . ? 
C10 C5 1.423(6) . ? 
C10 H10A 0.9700 . ? 
C10 H10B 0.9700 . ? 
C9 H9A 0.9600 . ? 
C9 H9B 0.9600 . ? 
C9 H9C 0.9600 . ? 
C8 H8A 0.9600 . ? 
C8 H8B 0.9600 . ? 
C8 H8C 0.9600 . ? 
C7 C2 1.469(7) . ? 
C7 H7A 0.9700 . ? 
C7 H7B 0.9700 . ? 
C6 H6A 0.9300 . ? 
C5 H5C 0.9700 . ? 
C5 H5D 0.9700 . ? 
C4 H4A 0.9300 . ? 
C3 H3A 0.9300 . ? 
C2 H2C 0.9700 . ? 
C2 H2D 0.9700 . ? 
C1 H1C 0.9300 . ? 
O1W C52 1.409(6) . ? 
C51 H51A 0.9600 . ? 
C51 H51B 0.9600 . ? 
C51 H51C 0.9600 . ? 
O2W C53 1.363(8) . ? 
O3W C54 1.548(11) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N11 Ni1 N10 91.95(10) . . ? 
N11 Ni1 N6 90.45(10) . . ? 
N10 Ni1 N6 90.51(10) . . ? 
N11 Ni1 N7 163.68(10) . . ? 
N10 Ni1 N7 99.54(10) . . ? 
N6 Ni1 N7 77.98(10) . . ? 
N11 Ni1 N12 77.64(10) . . ? 
N10 Ni1 N12 163.97(10) . . ? 
N6 Ni1 N12 101.60(10) . . ? 
N7 Ni1 N12 93.29(10) . . ? 
N11 Ni1 N9 102.58(10) . . ? 
N10 Ni1 N9 77.58(10) . . ? 
N6 Ni1 N9 162.51(10) . . ? 
N7 Ni1 N9 91.26(10) . . ? 
N12 Ni1 N9 92.66(9) . . ? 
O3 Ni2 O1 95.99(9) . . ? 
O3 Ni2 O2 96.58(9) . . ? 
O1 Ni2 O2 96.55(8) . . ? 
O3 Ni2 N8 169.96(10) . . ? 
O1 Ni2 N8 90.58(10) . . ? 
O2 Ni2 N8 90.20(10) . . ? 
O3 Ni2 N4 90.34(11) . . ? 
O1 Ni2 N4 90.24(11) . . ? 
O2 Ni2 N4 169.73(10) . . ? 
N8 Ni2 N4 82.01(12) . . ? 
O3 Ni2 N3 90.41(10) . . ? 
O1 Ni2 N3 169.68(10) . . ? 
O2 Ni2 N3 90.74(10) . . ? 
N8 Ni2 N3 82.07(11) . . ? 
N4 Ni2 N3 81.61(12) . . ? 
N10 O3 Ni2 110.82(16) . . ? 
N11 O2 Ni2 110.84(15) . . ? 
N6 O1 Ni2 110.48(16) . . ? 
C43 N12 C42 117.7(3) . . ? 
C43 N12 Ni1 129.2(2) . . ? 
C42 N12 Ni1 113.09(19) . . ? 
C44 N11 O2 116.7(2) . . ? 
C44 N11 Ni1 119.3(2) . . ? 
O2 N11 Ni1 123.92(17) . . ? 
C46 N10 O3 117.7(2) . . ? 
C46 N10 Ni1 118.0(2) . . ? 
O3 N10 Ni1 124.38(18) . . ? 
C40 N9 C47 118.7(3) . . ? 
C40 N9 Ni1 128.4(2) . . ? 
C47 N9 Ni1 112.1(2) . . ? 
C5 N8 C8 109.7(3) . . ? 
C5 N8 C24 113.5(3) . . ? 
C8 N8 C24 108.7(3) . . ? 
C5 N8 Ni2 109.1(2) . . ? 
C8 N8 Ni2 112.0(2) . . ? 
C24 N8 Ni2 103.8(2) . . ? 
C36 C50 C35 114.9(3) . . ? 
C36 C50 B1 124.5(3) . . ? 
C35 C50 B1 120.5(3) . . ? 
C41 N7 C45 117.8(3) . . ? 
C41 N7 Ni1 129.2(2) . . ? 
C45 N7 Ni1 112.9(2) . . ? 
C49 N6 O1 117.0(2) . . ? 
C49 N6 Ni1 117.5(2) . . ? 
O1 N6 Ni1 125.35(18) . . ? 
N6 C49 N1 123.3(3) . . ? 
N6 C49 C45 116.2(3) . . ? 
N1 C49 C45 120.5(3) . . ? 
C15 C48 C31 114.7(3) . . ? 
C15 C48 B1 122.9(3) . . ? 
C31 C48 B1 122.2(3) . . ? 
C44 N5 H5A 120.0 . . ? 
C44 N5 H5B 120.0 . . ? 
H5A N5 H5B 120.0 . . ? 
N9 C47 C14 120.9(3) . . ? 
N9 C47 C46 115.2(3) . . ? 
C14 C47 C46 123.9(3) . . ? 
C2 N4 C51 111.2(3) . . ? 
C2 N4 C10 111.0(4) . . ? 
C51 N4 C10 108.3(3) . . ? 
C2 N4 Ni2 110.6(3) . . ? 
C51 N4 Ni2 113.6(2) . . ? 
C10 N4 Ni2 101.8(2) . . ? 
N10 C46 N2 123.2(3) . . ? 
N10 C46 C47 115.9(3) . . ? 
N2 C46 C47 120.9(3) . . ? 
N7 C45 C25 121.5(3) . . ? 
N7 C45 C49 115.0(3) . . ? 
C25 C45 C49 123.4(3) . . ? 
N11 C44 N5 124.1(3) . . ? 
N11 C44 C42 115.3(3) . . ? 
N5 C44 C42 120.5(3) . . ? 
N12 C43 C29 123.5(3) . . ? 
N12 C43 H43A 118.2 . . ? 
C29 C43 H43A 118.2 . . ? 
N12 C42 C38 121.9(3) . . ? 
N12 C42 C44 114.5(3) . . ? 
C38 C42 C44 123.6(3) . . ? 
N7 C41 C12 123.5(4) . . ? 
N7 C41 H41A 118.2 . . ? 
C12 C41 H41A 118.2 . . ? 
C7 N3 C11 111.3(4) . . ? 
C7 N3 C9 109.4(3) . . ? 
C11 N3 C9 111.9(3) . . ? 
C7 N3 Ni2 102.5(2) . . ? 
C11 N3 Ni2 108.0(2) . . ? 
C9 N3 Ni2 113.4(2) . . ? 
C39 B1 C48 110.9(3) . . ? 
C39 B1 C37 114.2(3) . . ? 
C48 B1 C37 103.9(3) . . ? 
C39 B1 C50 105.1(3) . . ? 
C48 B1 C50 112.4(3) . . ? 
C37 B1 C50 110.4(3) . . ? 
N9 C40 C32 122.8(3) . . ? 
N9 C40 H40A 118.6 . . ? 
C32 C40 H40A 118.6 . . ? 
C23 C39 C21 114.3(3) . . ? 
C23 C39 B1 125.2(3) . . ? 
C21 C39 B1 120.4(3) . . ? 
C42 C38 C26 119.1(3) . . ? 
C42 C38 H38A 120.4 . . ? 
C26 C38 H38A 120.4 . . ? 
C30 C37 C34 114.8(3) . . ? 
C30 C37 B1 121.8(3) . . ? 
C34 C37 B1 123.0(3) . . ? 
C46 N2 H2A 120.0 . . ? 
C46 N2 H2B 120.0 . . ? 
H2A N2 H2B 120.0 . . ? 
C50 C36 C27 122.7(3) . . ? 
C50 C36 H36A 118.7 . . ? 
C27 C36 H36A 118.7 . . ? 
C18 C35 C50 122.5(4) . . ? 
C18 C35 H35A 118.7 . . ? 
C50 C35 H35A 118.7 . . ? 
C33 C34 C37 122.3(4) . . ? 
C33 C34 H34A 118.9 . . ? 
C37 C34 H34A 118.9 . . ? 
C22 C33 C34 120.8(4) . . ? 
C22 C33 H33A 119.6 . . ? 
C34 C33 H33A 119.6 . . ? 
C1 C32 C40 118.4(4) . . ? 
C1 C32 H32A 120.8 . . ? 
C40 C32 H32A 120.8 . . ? 
C3 C31 C48 122.6(4) . . ? 
C3 C31 H31A 118.7 . . ? 
C48 C31 H31A 118.7 . . ? 
C37 C30 C19 123.1(3) . . ? 
C37 C30 H30A 118.4 . . ? 
C19 C30 H30A 118.4 . . ? 
C26 C29 C43 118.6(3) . . ? 
C26 C29 H29A 120.7 . . ? 
C43 C29 H29A 120.7 . . ? 
C27 C28 C18 119.2(4) . . ? 
C27 C28 H28A 120.4 . . ? 
C18 C28 H28A 120.4 . . ? 
C49 N1 H1A 120.0 . . ? 
C49 N1 H1B 120.0 . . ? 
H1A N1 H1B 120.0 . . ? 
C28 C27 C36 120.5(4) . . ? 
C28 C27 H27A 119.8 . . ? 
C36 C27 H27A 119.8 . . ? 
C29 C26 C38 119.3(3) . . ? 
C29 C26 H26A 120.4 . . ? 
C38 C26 H26A 120.4 . . ? 
C6 C25 C45 119.2(4) . . ? 
C6 C25 H25A 120.4 . . ? 
C45 C25 H25A 120.4 . . ? 
C11 C24 N8 113.5(4) . . ? 
C11 C24 H24A 108.9 . . ? 
N8 C24 H24A 108.9 . . ? 
C11 C24 H24B 108.9 . . ? 
N8 C24 H24B 108.9 . . ? 
H24A C24 H24B 107.7 . . ? 
C39 C23 C4 122.6(4) . . ? 
C39 C23 H23A 118.7 . . ? 
C4 C23 H23A 118.7 . . ? 
C33 C22 C19 119.6(4) . . ? 
C33 C22 H22A 120.2 . . ? 
C19 C22 H22A 120.2 . . ? 
C17 C21 C39 123.7(4) . . ? 
C17 C21 H21A 118.1 . . ? 
C39 C21 H21A 118.1 . . ? 
C3 C20 C16 118.5(4) . . ? 
C3 C20 H20A 120.7 . . ? 
C16 C20 H20A 120.7 . . ? 
C22 C19 C30 119.4(4) . . ? 
C22 C19 H19A 120.3 . . ? 
C30 C19 H19A 120.3 . . ? 
C28 C18 C35 120.2(4) . . ? 
C28 C18 H18A 119.9 . . ? 
C35 C18 H18A 119.9 . . ? 
C13 C17 C21 120.1(4) . . ? 
C13 C17 H17A 120.0 . . ? 
C21 C17 H17A 120.0 . . ? 
C15 C16 C20 119.7(4) . . ? 
C15 C16 H16A 120.2 . . ? 
C20 C16 H16A 120.2 . . ? 
C16 C15 C48 123.9(4) . . ? 
C16 C15 H15A 118.1 . . ? 
C48 C15 H15A 118.1 . . ? 
C1 C14 C47 119.5(4) . . ? 
C1 C14 H14A 120.2 . . ? 
C47 C14 H14A 120.2 . . ? 
C17 C13 C4 118.7(4) . . ? 
C17 C13 H13A 120.6 . . ? 
C4 C13 H13A 120.6 . . ? 
C6 C12 C41 117.8(4) . . ? 
C6 C12 H12A 121.1 . . ? 
C41 C12 H12A 121.1 . . ? 
C24 C11 N3 114.4(3) . . ? 
C24 C11 H11A 108.6 . . ? 
N3 C11 H11A 108.6 . . ? 
C24 C11 H11B 108.6 . . ? 
N3 C11 H11B 108.6 . . ? 
H11A C11 H11B 107.6 . . ? 
C5 C10 N4 114.2(4) . . ? 
C5 C10 H10A 108.7 . . ? 
N4 C10 H10A 108.7 . . ? 
C5 C10 H10B 108.7 . . ? 
N4 C10 H10B 108.7 . . ? 
H10A C10 H10B 107.6 . . ? 
N3 C9 H9A 109.5 . . ? 
N3 C9 H9B 109.5 . . ? 
H9A C9 H9B 109.5 . . ? 
N3 C9 H9C 109.5 . . ? 
H9A C9 H9C 109.5 . . ? 
H9B C9 H9C 109.5 . . ? 
N8 C8 H8A 109.5 . . ? 
N8 C8 H8B 109.5 . . ? 
H8A C8 H8B 109.5 . . ? 
N8 C8 H8C 109.5 . . ? 
H8A C8 H8C 109.5 . . ? 
H8B C8 H8C 109.5 . . ? 
C2 C7 N3 115.5(4) . . ? 
C2 C7 H7A 108.4 . . ? 
N3 C7 H7A 108.4 . . ? 
C2 C7 H7B 108.4 . . ? 
N3 C7 H7B 108.4 . . ? 
H7A C7 H7B 107.5 . . ? 
C12 C6 C25 120.1(4) . . ? 
C12 C6 H6A 119.9 . . ? 
C25 C6 H6A 119.9 . . ? 
C10 C5 N8 114.6(4) . . ? 
C10 C5 H5C 108.6 . . ? 
N8 C5 H5C 108.6 . . ? 
C10 C5 H5D 108.6 . . ? 
N8 C5 H5D 108.6 . . ? 
H5C C5 H5D 107.6 . . ? 
C13 C4 C23 120.6(4) . . ? 
C13 C4 H4A 119.7 . . ? 
C23 C4 H4A 119.7 . . ? 
C20 C3 C31 120.6(5) . . ? 
C20 C3 H3A 119.7 . . ? 
C31 C3 H3A 119.7 . . ? 
N4 C2 C7 111.8(4) . . ? 
N4 C2 H2C 109.3 . . ? 
C7 C2 H2C 109.3 . . ? 
N4 C2 H2D 109.3 . . ? 
C7 C2 H2D 109.3 . . ? 
H2C C2 H2D 107.9 . . ? 
C14 C1 C32 119.8(4) . . ? 
C14 C1 H1C 120.1 . . ? 
C32 C1 H1C 120.1 . . ? 
N4 C51 H51A 109.5 . . ? 
N4 C51 H51B 109.5 . . ? 
H51A C51 H51B 109.5 . . ? 
N4 C51 H51C 109.5 . . ? 
H51A C51 H51C 109.5 . . ? 
H51B C51 H51C 109.5 . . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
O1 Ni2 O3 N10 70.33(18) . . . . ? 
O2 Ni2 O3 N10 -27.00(18) . . . . ? 
N8 Ni2 O3 N10 -159.1(5) . . . . ? 
N4 Ni2 O3 N10 160.60(19) . . . . ? 
N3 Ni2 O3 N10 -117.79(18) . . . . ? 
O3 Ni2 O2 N11 69.59(18) . . . . ? 
O1 Ni2 O2 N11 -27.24(18) . . . . ? 
N8 Ni2 O2 N11 -117.84(18) . . . . ? 
N4 Ni2 O2 N11 -158.3(6) . . . . ? 
N3 Ni2 O2 N11 160.09(19) . . . . ? 
O3 Ni2 O1 N6 -29.43(18) . . . . ? 
O2 Ni2 O1 N6 67.92(18) . . . . ? 
N8 Ni2 O1 N6 158.19(18) . . . . ? 
N4 Ni2 O1 N6 -119.80(19) . . . . ? 
N3 Ni2 O1 N6 -157.4(5) . . . . ? 
N11 Ni1 N12 C43 -179.0(3) . . . . ? 
N10 Ni1 N12 C43 130.5(4) . . . . ? 
N6 Ni1 N12 C43 -91.1(3) . . . . ? 
N7 Ni1 N12 C43 -12.8(3) . . . . ? 
N9 Ni1 N12 C43 78.7(3) . . . . ? 
N11 Ni1 N12 C42 4.35(19) . . . . ? 
N10 Ni1 N12 C42 -46.1(4) . . . . ? 
N6 Ni1 N12 C42 92.2(2) . . . . ? 
N7 Ni1 N12 C42 170.6(2) . . . . ? 
N9 Ni1 N12 C42 -97.9(2) . . . . ? 
Ni2 O2 N11 C44 136.4(2) . . . . ? 
Ni2 O2 N11 Ni1 -40.9(2) . . . . ? 
N10 Ni1 N11 C44 164.4(2) . . . . ? 
N6 Ni1 N11 C44 -105.1(2) . . . . ? 
N7 Ni1 N11 C44 -60.7(5) . . . . ? 
N12 Ni1 N11 C44 -3.3(2) . . . . ? 
N9 Ni1 N11 C44 86.7(2) . . . . ? 
N10 Ni1 N11 O2 -18.3(2) . . . . ? 
N6 Ni1 N11 O2 72.2(2) . . . . ? 
N7 Ni1 N11 O2 116.6(4) . . . . ? 
N12 Ni1 N11 O2 174.0(2) . . . . ? 
N9 Ni1 N11 O2 -96.0(2) . . . . ? 
Ni2 O3 N10 C46 140.3(2) . . . . ? 
Ni2 O3 N10 Ni1 -39.6(2) . . . . ? 
N11 Ni1 N10 C46 -109.4(2) . . . . ? 
N6 Ni1 N10 C46 160.1(2) . . . . ? 
N7 Ni1 N10 C46 82.2(2) . . . . ? 
N12 Ni1 N10 C46 -60.5(5) . . . . ? 
N9 Ni1 N10 C46 -6.9(2) . . . . ? 
N11 Ni1 N10 O3 70.5(2) . . . . ? 
N6 Ni1 N10 O3 -19.9(2) . . . . ? 
N7 Ni1 N10 O3 -97.8(2) . . . . ? 
N12 Ni1 N10 O3 119.5(3) . . . . ? 
N9 Ni1 N10 O3 173.0(2) . . . . ? 
N11 Ni1 N9 C40 -91.5(3) . . . . ? 
N10 Ni1 N9 C40 179.3(3) . . . . ? 
N6 Ni1 N9 C40 131.3(3) . . . . ? 
N7 Ni1 N9 C40 79.8(3) . . . . ? 
N12 Ni1 N9 C40 -13.5(3) . . . . ? 
N11 Ni1 N9 C47 99.0(2) . . . . ? 
N10 Ni1 N9 C47 9.8(2) . . . . ? 
N6 Ni1 N9 C47 -38.3(4) . . . . ? 
N7 Ni1 N9 C47 -89.7(2) . . . . ? 
N12 Ni1 N9 C47 176.9(2) . . . . ? 
O3 Ni2 N8 C5 -51.2(7) . . . . ? 
O1 Ni2 N8 C5 79.7(3) . . . . ? 
O2 Ni2 N8 C5 176.3(3) . . . . ? 
N4 Ni2 N8 C5 -10.5(3) . . . . ? 
N3 Ni2 N8 C5 -93.0(3) . . . . ? 
O3 Ni2 N8 C8 -172.9(5) . . . . ? 
O1 Ni2 N8 C8 -42.0(2) . . . . ? 
O2 Ni2 N8 C8 54.6(2) . . . . ? 
N4 Ni2 N8 C8 -132.1(3) . . . . ? 
N3 Ni2 N8 C8 145.3(3) . . . . ? 
O3 Ni2 N8 C24 70.1(7) . . . . ? 
O1 Ni2 N8 C24 -159.0(3) . . . . ? 
O2 Ni2 N8 C24 -62.4(3) . . . . ? 
N4 Ni2 N8 C24 110.8(3) . . . . ? 
N3 Ni2 N8 C24 28.3(3) . . . . ? 
N11 Ni1 N7 C41 137.4(4) . . . . ? 
N10 Ni1 N7 C41 -88.4(3) . . . . ? 
N6 Ni1 N7 C41 -176.9(3) . . . . ? 
N12 Ni1 N7 C41 81.9(3) . . . . ? 
N9 Ni1 N7 C41 -10.8(3) . . . . ? 
N11 Ni1 N7 C45 -39.5(5) . . . . ? 
N10 Ni1 N7 C45 94.7(2) . . . . ? 
N6 Ni1 N7 C45 6.2(2) . . . . ? 
N12 Ni1 N7 C45 -95.0(2) . . . . ? 
N9 Ni1 N7 C45 172.3(2) . . . . ? 
Ni2 O1 N6 C49 136.0(2) . . . . ? 
Ni2 O1 N6 Ni1 -38.3(2) . . . . ? 
N11 Ni1 N6 C49 164.4(2) . . . . ? 
N10 Ni1 N6 C49 -103.6(2) . . . . ? 
N7 Ni1 N6 C49 -4.0(2) . . . . ? 
N12 Ni1 N6 C49 87.0(2) . . . . ? 
N9 Ni1 N6 C49 -57.0(4) . . . . ? 
N11 Ni1 N6 O1 -21.3(2) . . . . ? 
N10 Ni1 N6 O1 70.7(2) . . . . ? 
N7 Ni1 N6 O1 170.3(2) . . . . ? 
N12 Ni1 N6 O1 -98.7(2) . . . . ? 
N9 Ni1 N6 O1 117.3(3) . . . . ? 
O1 N6 C49 N1 5.1(5) . . . . ? 
Ni1 N6 C49 N1 179.9(3) . . . . ? 
O1 N6 C49 C45 -173.6(3) . . . . ? 
Ni1 N6 C49 C45 1.2(4) . . . . ? 
C40 N9 C47 C14 0.6(5) . . . . ? 
Ni1 N9 C47 C14 171.3(3) . . . . ? 
C40 N9 C47 C46 178.0(3) . . . . ? 
Ni1 N9 C47 C46 -11.3(3) . . . . ? 
O3 Ni2 N4 C2 84.3(3) . . . . ? 
O1 Ni2 N4 C2 -179.7(3) . . . . ? 
O2 Ni2 N4 C2 -48.2(8) . . . . ? 
N8 Ni2 N4 C2 -89.1(3) . . . . ? 
N3 Ni2 N4 C2 -6.0(3) . . . . ? 
O3 Ni2 N4 C51 -41.5(3) . . . . ? 
O1 Ni2 N4 C51 54.5(3) . . . . ? 
O2 Ni2 N4 C51 -174.0(5) . . . . ? 
N8 Ni2 N4 C51 145.0(3) . . . . ? 
N3 Ni2 N4 C51 -131.9(3) . . . . ? 
O3 Ni2 N4 C10 -157.7(3) . . . . ? 
O1 Ni2 N4 C10 -61.7(3) . . . . ? 
O2 Ni2 N4 C10 69.8(7) . . . . ? 
N8 Ni2 N4 C10 28.8(3) . . . . ? 
N3 Ni2 N4 C10 111.9(3) . . . . ? 
O3 N10 C46 N2 2.2(5) . . . . ? 
Ni1 N10 C46 N2 -177.9(3) . . . . ? 
O3 N10 C46 C47 -177.0(3) . . . . ? 
Ni1 N10 C46 C47 2.9(4) . . . . ? 
N9 C47 C46 N10 6.1(4) . . . . ? 
C14 C47 C46 N10 -176.7(4) . . . . ? 
N9 C47 C46 N2 -173.1(3) . . . . ? 
C14 C47 C46 N2 4.2(5) . . . . ? 
C41 N7 C45 C25 -1.0(5) . . . . ? 
Ni1 N7 C45 C25 176.2(3) . . . . ? 
C41 N7 C45 C49 175.3(3) . . . . ? 
Ni1 N7 C45 C49 -7.5(4) . . . . ? 
N6 C49 C45 N7 4.4(4) . . . . ? 
N1 C49 C45 N7 -174.3(3) . . . . ? 
N6 C49 C45 C25 -179.3(3) . . . . ? 
N1 C49 C45 C25 1.9(5) . . . . ? 
O2 N11 C44 N5 0.5(4) . . . . ? 
Ni1 N11 C44 N5 178.0(2) . . . . ? 
O2 N11 C44 C42 -175.8(2) . . . . ? 
Ni1 N11 C44 C42 1.7(4) . . . . ? 
C42 N12 C43 C29 -0.6(4) . . . . ? 
Ni1 N12 C43 C29 -177.1(2) . . . . ? 
C43 N12 C42 C38 0.6(4) . . . . ? 
Ni1 N12 C42 C38 177.7(2) . . . . ? 
C43 N12 C42 C44 178.2(3) . . . . ? 
Ni1 N12 C42 C44 -4.8(3) . . . . ? 
N11 C44 C42 N12 2.3(4) . . . . ? 
N5 C44 C42 N12 -174.2(3) . . . . ? 
N11 C44 C42 C38 179.8(3) . . . . ? 
N5 C44 C42 C38 3.3(5) . . . . ? 
C45 N7 C41 C12 -0.1(5) . . . . ? 
Ni1 N7 C41 C12 -176.8(3) . . . . ? 
O3 Ni2 N3 C7 -64.0(3) . . . . ? 
O1 Ni2 N3 C7 64.4(6) . . . . ? 
O2 Ni2 N3 C7 -160.6(2) . . . . ? 
N8 Ni2 N3 C7 109.3(3) . . . . ? 
N4 Ni2 N3 C7 26.3(3) . . . . ? 
O3 Ni2 N3 C11 178.4(3) . . . . ? 
O1 Ni2 N3 C11 -53.2(7) . . . . ? 
O2 Ni2 N3 C11 81.8(3) . . . . ? 
N8 Ni2 N3 C11 -8.3(3) . . . . ? 
N4 Ni2 N3 C11 -91.3(3) . . . . ? 
O3 Ni2 N3 C9 53.8(3) . . . . ? 
O1 Ni2 N3 C9 -177.8(5) . . . . ? 
O2 Ni2 N3 C9 -42.8(3) . . . . ? 
N8 Ni2 N3 C9 -132.9(3) . . . . ? 
N4 Ni2 N3 C9 144.1(3) . . . . ? 
C15 C48 B1 C39 156.2(3) . . . . ? 
C31 C48 B1 C39 -29.0(4) . . . . ? 
C15 C48 B1 C37 -80.7(4) . . . . ? 
C31 C48 B1 C37 94.2(4) . . . . ? 
C15 C48 B1 C50 38.8(4) . . . . ? 
C31 C48 B1 C50 -146.4(3) . . . . ? 
C36 C50 B1 C39 -99.0(4) . . . . ? 
C35 C50 B1 C39 77.1(4) . . . . ? 
C36 C50 B1 C48 21.7(4) . . . . ? 
C35 C50 B1 C48 -162.1(3) . . . . ? 
C36 C50 B1 C37 137.3(3) . . . . ? 
C35 C50 B1 C37 -46.5(4) . . . . ? 
C47 N9 C40 C32 0.3(5) . . . . ? 
Ni1 N9 C40 C32 -168.6(3) . . . . ? 
C48 B1 C39 C23 140.2(3) . . . . ? 
C37 B1 C39 C23 23.1(4) . . . . ? 
C50 B1 C39 C23 -98.0(4) . . . . ? 
C48 B1 C39 C21 -43.9(4) . . . . ? 
C37 B1 C39 C21 -160.9(3) . . . . ? 
C50 B1 C39 C21 77.9(4) . . . . ? 
N12 C42 C38 C26 -0.7(5) . . . . ? 
C44 C42 C38 C26 -178.0(3) . . . . ? 
C39 B1 C37 C30 -148.3(3) . . . . ? 
C48 B1 C37 C30 90.7(3) . . . . ? 
C50 B1 C37 C30 -30.1(4) . . . . ? 
C39 B1 C37 C34 39.2(4) . . . . ? 
C48 B1 C37 C34 -81.8(4) . . . . ? 
C50 B1 C37 C34 157.4(3) . . . . ? 
C35 C50 C36 C27 1.3(5) . . . . ? 
B1 C50 C36 C27 177.7(3) . . . . ? 
C36 C50 C35 C18 -1.1(5) . . . . ? 
B1 C50 C35 C18 -177.6(4) . . . . ? 
C30 C37 C34 C33 1.1(5) . . . . ? 
B1 C37 C34 C33 174.2(4) . . . . ? 
C37 C34 C33 C22 -1.2(6) . . . . ? 
N9 C40 C32 C1 0.1(6) . . . . ? 
C15 C48 C31 C3 -1.3(6) . . . . ? 
B1 C48 C31 C3 -176.5(4) . . . . ? 
C34 C37 C30 C19 -0.3(5) . . . . ? 
B1 C37 C30 C19 -173.4(3) . . . . ? 
N12 C43 C29 C26 0.7(5) . . . . ? 
C18 C28 C27 C36 -1.2(6) . . . . ? 
C50 C36 C27 C28 -0.2(6) . . . . ? 
C43 C29 C26 C38 -0.8(5) . . . . ? 
C42 C38 C26 C29 0.8(5) . . . . ? 
N7 C45 C25 C6 1.9(6) . . . . ? 
C49 C45 C25 C6 -174.0(4) . . . . ? 
C5 N8 C24 C11 72.0(5) . . . . ? 
C8 N8 C24 C11 -165.7(4) . . . . ? 
Ni2 N8 C24 C11 -46.3(5) . . . . ? 
C21 C39 C23 C4 1.7(5) . . . . ? 
B1 C39 C23 C4 177.9(4) . . . . ? 
C34 C33 C22 C19 0.4(6) . . . . ? 
C23 C39 C21 C17 -1.0(6) . . . . ? 
B1 C39 C21 C17 -177.3(4) . . . . ? 
C33 C22 C19 C30 0.4(6) . . . . ? 
C37 C30 C19 C22 -0.5(6) . . . . ? 
C27 C28 C18 C35 1.4(6) . . . . ? 
C50 C35 C18 C28 -0.2(7) . . . . ? 
C39 C21 C17 C13 -0.3(7) . . . . ? 
C3 C20 C16 C15 -0.1(7) . . . . ? 
C20 C16 C15 C48 -1.4(6) . . . . ? 
C31 C48 C15 C16 2.0(5) . . . . ? 
B1 C48 C15 C16 177.2(3) . . . . ? 
N9 C47 C14 C1 -2.0(6) . . . . ? 
C46 C47 C14 C1 -179.1(4) . . . . ? 
C21 C17 C13 C4 0.9(7) . . . . ? 
N7 C41 C12 C6 0.3(6) . . . . ? 
N8 C24 C11 N3 43.0(6) . . . . ? 
C7 N3 C11 C24 -126.7(5) . . . . ? 
C9 N3 C11 C24 110.5(5) . . . . ? 
Ni2 N3 C11 C24 -15.0(5) . . . . ? 
C2 N4 C10 C5 71.1(5) . . . . ? 
C51 N4 C10 C5 -166.6(4) . . . . ? 
Ni2 N4 C10 C5 -46.6(5) . . . . ? 
C11 N3 C7 C2 69.0(5) . . . . ? 
C9 N3 C7 C2 -166.7(4) . . . . ? 
Ni2 N3 C7 C2 -46.1(5) . . . . ? 
C41 C12 C6 C25 0.7(7) . . . . ? 
C45 C25 C6 C12 -1.7(7) . . . . ? 
N4 C10 C5 N8 42.2(6) . . . . ? 
C8 N8 C5 C10 110.0(4) . . . . ? 
C24 N8 C5 C10 -128.2(5) . . . . ? 
Ni2 N8 C5 C10 -13.1(5) . . . . ? 
C17 C13 C4 C23 -0.1(7) . . . . ? 
C39 C23 C4 C13 -1.2(7) . . . . ? 
C16 C20 C3 C31 0.7(7) . . . . ? 
C48 C31 C3 C20 -0.1(7) . . . . ? 
C51 N4 C2 C7 110.3(5) . . . . ? 
C10 N4 C2 C7 -129.1(5) . . . . ? 
Ni2 N4 C2 C7 -16.9(5) . . . . ? 
N3 C7 C2 N4 44.6(6) . . . . ? 
C47 C14 C1 C32 2.4(8) . . . . ? 
C40 C32 C1 C14 -1.5(7) . . . . ? 
 
_diffrn_measured_fraction_theta_max    0.987 
_diffrn_reflns_theta_full              27.46 
_diffrn_measured_fraction_theta_full   0.987 
_refine_diff_density_max    0.612 
_refine_diff_density_min   -0.614 
_refine_diff_density_rms    0.065  

#===End

data_4 
  
_audit_creation_method            SHELXL-97 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_melting_point           ? 
_chemical_formula_moiety          ? 
_chemical_formula_sum 
 'C52 H76 Cl2 N26 Ni5 O19' 
_chemical_formula_weight          1733.84 
  
loop_ 
 _atom_type_symbol 
 _atom_type_description 
 _atom_type_scat_dispersion_real 
 _atom_type_scat_dispersion_imag 
 _atom_type_scat_source 
 'C'  'C'   0.0033   0.0016 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'H'  'H'   0.0000   0.0000 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'N'  'N'   0.0061   0.0033 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'O'  'O'   0.0106   0.0060 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Ni'  'Ni'   0.3393   1.1124 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
 'Cl'  'Cl'   0.1484   0.1585 
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
  
_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    'C 2/c' 
  
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, y, -z+1/2' 
 'x+1/2, y+1/2, z' 
 '-x+1/2, y+1/2, -z+1/2' 
 '-x, -y, -z' 
 'x, -y, z-1/2' 
 '-x+1/2, -y+1/2, -z' 
 'x+1/2, -y+1/2, z-1/2' 
  
_cell_length_a                    18.717(6)
_cell_length_b                    25.333(8)
_cell_length_c                    17.423(5)
_cell_angle_alpha                 90
_cell_angle_beta                  99.435(6)
_cell_angle_gamma                 90
_cell_volume                      8150(4)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     8924 
_cell_measurement_theta_min       3.12 
_cell_measurement_theta_max       27.5 
  
_exptl_crystal_description        block
_exptl_crystal_colour             'dark red' 
_exptl_crystal_size_max           0.22 
_exptl_crystal_size_mid           0.18 
_exptl_crystal_size_min           0.10 
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.413 
_exptl_crystal_density_method     'not measured' 
_exptl_crystal_F_000              3584 
_exptl_absorpt_coefficient_mu     1.275 
_exptl_absorpt_correction_type    empirical 
_exptl_absorpt_correction_T_min   0.399 
_exptl_absorpt_correction_T_max   1.000
_exptl_absorpt_process_details    'ABSCOR; T Higashi (2001)'
  
_exptl_special_details 
; 
 ? 
; 
  
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_measurement_device_type   'Rigaku R-AXIS RAPID IP' 
_diffrn_measurement_method        'ω scans' 
_diffrn_detector_area_resol_mean  0.77 
_diffrn_standards_decay_%         ? 
_diffrn_reflns_number             37761 
_diffrn_reflns_av_R_equivalents   0.0746 
_diffrn_reflns_av_sigmaI/netI     0.0667 
_diffrn_reflns_limit_h_min        -23 
_diffrn_reflns_limit_h_max        24 
_diffrn_reflns_limit_k_min        -32 
_diffrn_reflns_limit_k_max        32 
_diffrn_reflns_limit_l_min        -22 
_diffrn_reflns_limit_l_max        21 
_diffrn_reflns_theta_min          3.12 
_diffrn_reflns_theta_max          27.48 
_reflns_number_total              9052 
_reflns_number_gt                 5405 
_reflns_threshold_expression      >2sigma(I) 
  
_computing_data_collection        'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_cell_refinement        'crystalstructure 3.6.0 (Rigaku, 2004)'
_computing_data_reduction         'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)' 
_computing_molecular_graphics     'XP (Sheldrick, 1998)' 
_computing_publication_material   'XP (Sheldrick, 1998)' 
  
_refine_special_details 
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
; 
 

_refine_ls_structure_factor_coef  Fsqd 
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme       calc 
_refine_ls_weighting_details 
 'calc w=1/[σ²(Fo²)+(0.1734P)²+0.0000P] where P=(Fo²+2Fc²)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     constr 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          9052 
_refine_ls_number_parameters      475 
_refine_ls_number_restraints      27 
_refine_ls_R_factor_all           0.1120 
_refine_ls_R_factor_gt            0.0762 
_refine_ls_wR_factor_ref          0.2690 
_refine_ls_wR_factor_gt           0.2229 
_refine_ls_goodness_of_fit_ref    1.023 
_refine_ls_restrained_S_all       1.025 
_refine_ls_shift/su_max           0.001 
_refine_ls_shift/su_mean          0.000 
 
loop_ 
 _atom_site_label 
 _atom_site_type_symbol 
 _atom_site_fract_x 
 _atom_site_fract_y 
 _atom_site_fract_z 
 _atom_site_U_iso_or_equiv 
 _atom_site_adp_type 
 _atom_site_occupancy 
 _atom_site_symmetry_multiplicity 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_assembly 
 _atom_site_disorder_group 
Ni1 Ni 0.5000 0.35169(3) 0.2500 0.0518(3) Uani 1 2 d S . . 
Cl1 Cl 0.15715(10) 0.20218(7) 0.37557(9) 0.0840(5) Uani 1 1 d . . . 
Ni2 Ni 0.75504(4) 0.35089(3) 0.34326(4) 0.0601(2) Uani 1 1 d . . . 
Ni3 Ni 0.63503(3) 0.43069(3) 0.40625(3) 0.0566(2) Uani 1 1 d . . . 
C1 C 0.6454(3) 0.3087(2) 0.2492(3) 0.0579(11) Uani 1 1 d . . . 
C2 C 0.5995(3) 0.2792(2) 0.1857(3) 0.0618(12) Uani 1 1 d . . . 
C3 C 0.5100(3) 0.3848(2) 0.4550(3) 0.0607(12) Uani 1 1 d . . . 
C5 C 0.4833(3) 0.2687(2) 0.1196(3) 0.0741(15) Uani 1 1 d . . . 
H5A H 0.4343 0.2771 0.1129 0.089 Uiso 1 1 calc R . . 
C6 C 0.5067(4) 0.2329(3) 0.0712(4) 0.093(2) Uani 1 1 d . . . 
H6C H 0.4736 0.2172 0.0323 0.112 Uiso 1 1 calc R . . 
C7 C 0.6252(4) 0.2429(3) 0.1391(4) 0.0885(19) Uani 1 1 d . . . 
H7A H 0.6740 0.2337 0.1474 0.106 Uiso 1 1 calc R . . 
C8 C 0.5772(4) 0.2199(3) 0.0791(4) 0.101(2) Uani 1 1 d . . . 
H8A H 0.5935 0.1962 0.0451 0.122 Uiso 1 1 calc R . . 
C9 C 0.8879(4) 0.2960(3) 0.3235(4) 0.0888(19) Uani 1 1 d . . . 
H9C H 0.8594 0.2720 0.2917 0.107 Uiso 1 1 calc R . . 
C10 C 0.9598(4) 0.2893(3) 0.3361(5) 0.097(2) Uani 1 1 d . . . 
H10B H 0.9808 0.2608 0.3147 0.117 Uiso 1 1 calc R . . 
C11 C 1.0028(4) 0.3267(4) 0.3826(5) 0.098(2) Uani 1 1 d . . . 
H11A H 1.0530 0.3234 0.3913 0.118 Uiso 1 1 calc R . . 
C12 C 0.9712(3) 0.3670(3) 0.4143(4) 0.0870(18) Uani 1 1 d . . . 
H12A H 0.9994 0.3919 0.4447 0.104 Uiso 1 1 calc R . . 
C13 C 0.8971(3) 0.3711(3) 0.4015(3) 0.0744(15) Uani 1 1 d . . . 
C14 C 0.8544(3) 0.4112(2) 0.4331(4) 0.0739(15) Uani 1 1 d . . . 
C15 C 0.5667(3) 0.3756(2) 0.5234(3) 0.0646(13) Uani 1 1 d . . . 
C16 C 0.5547(4) 0.3548(3) 0.5932(3) 0.0822(18) Uani 1 1 d . . . 
H16A H 0.5080 0.3469 0.6012 0.099 Uiso 1 1 calc R . . 
C17 C 0.6125(5) 0.3459(3) 0.6503(4) 0.097(2) Uani 1 1 d . . . 
H17A H 0.6052 0.3304 0.6967 0.116 Uiso 1 1 calc R . . 
C18 C 0.6807(5) 0.3594(3) 0.6402(4) 0.099(2) Uani 1 1 d . . . 
H18A H 0.7204 0.3535 0.6788 0.118 Uiso 1 1 calc R . . 
C19 C 0.6883(4) 0.3823(3) 0.5695(3) 0.0827(17) Uani 1 1 d . . . 
H19A H 0.7344 0.3925 0.5623 0.099 Uiso 1 1 calc R . . 
C20 C 0.5933(6) 0.5390(3) 0.3982(4) 0.131(4) Uani 1 1 d . . . 
H20A H 0.5413 0.5417 0.3960 0.158 Uiso 1 1 calc R . . 
H20B H 0.6135 0.5733 0.4139 0.158 Uiso 1 1 calc R . . 
C21 C 0.6055(6) 0.5302(3) 0.3234(4) 0.114(3) Uani 1 1 d . . . 
H21A H 0.6477 0.5504 0.3157 0.136 Uiso 1 1 calc R . . 
H21B H 0.5645 0.5439 0.2877 0.136 Uiso 1 1 calc R . . 
C22 C 0.6726(4) 0.4714(3) 0.2533(3) 0.0885(19) Uani 1 1 d . . . 
H22A H 0.6786 0.4342 0.2427 0.106 Uiso 1 1 calc R . . 
H22B H 0.7178 0.4835 0.2835 0.106 Uiso 1 1 calc R . . 
C23 C 0.6623(4) 0.4999(3) 0.1772(4) 0.0886(19) Uani 1 1 d . . . 
H23A H 0.6638 0.5375 0.1874 0.106 Uiso 1 1 calc R . . 
H23B H 0.7028 0.4915 0.1510 0.106 Uiso 1 1 calc R . . 
C29 C 1.0952(9) 0.4312(6) 0.6078(10) 0.192(6) Uani 1 1 d . . . 
C30 C 1.1739(8) 0.4292(8) 0.6344(13) 0.247(9) Uani 1 1 d . . . 
C31 C 0.2401(8) 0.3682(6) 0.4030(9) 0.197(6) Uani 1 1 d D . . 
H31A H 0.2204 0.3339 0.4098 0.296 Uiso 1 1 calc R . . 
H31B H 0.2883 0.3704 0.4321 0.296 Uiso 1 1 calc R . . 
H31C H 0.2416 0.3740 0.3488 0.296 Uiso 1 1 calc R . . 
C32 C 0.1955(10) 0.4077(8) 0.4304(12) 0.244(9) Uani 1 1 d D . . 
N1 N 0.6105(2) 0.34213(17) 0.2870(2) 0.0564(9) Uani 1 1 d . . . 
N2 N 0.5307(2) 0.40557(16) 0.3949(2) 0.0562(9) Uani 1 1 d . . . 
N3 N 0.7168(2) 0.30291(18) 0.2680(3) 0.0672(11) Uani 1 1 d . . . 
H3A H 0.7418 0.2799 0.2477 0.081 Uiso 1 1 calc R . . 
N4 N 0.5279(2) 0.29183(17) 0.1758(2) 0.0577(10) Uani 1 1 d . . . 
N5 N 0.7856(2) 0.40695(19) 0.4096(3) 0.0650(11) Uani 1 1 d . . . 
N6 N 0.8848(3) 0.4511(3) 0.4791(4) 0.1036(19) Uani 1 1 d . . . 
H6A H 0.8579 0.4752 0.4942 0.124 Uiso 1 1 calc R . . 
H6B H 0.9310 0.4522 0.4933 0.124 Uiso 1 1 calc R . . 
N7 N 0.6337(3) 0.39041(18) 0.5117(2) 0.0666(11) Uani 1 1 d . . . 
N8 N 0.6169(2) 0.47580(17) 0.3023(2) 0.0580(10) Uani 1 1 d . . . 
H8B H 0.5747 0.4642 0.2738 0.070 Uiso 1 1 calc R . . 
N9 N 0.4398(3) 0.3703(2) 0.4569(3) 0.0761(13) Uani 1 1 d . . . 
H9A H 0.4072 0.3749 0.4166 0.091 Uiso 1 1 calc R . . 
H9B H 0.4285 0.3565 0.4984 0.091 Uiso 1 1 calc R . . 
N10 N 0.6191(3) 0.5033(2) 0.4579(3) 0.0782(13) Uani 1 1 d . . . 
H10A H 0.5868 0.4999 0.4905 0.094 Uiso 1 1 calc R . . 
H10C H 0.6611 0.5151 0.4852 0.094 Uiso 1 1 calc R . . 
N11 N 0.8552(3) 0.3360(2) 0.3547(3) 0.0713(12) Uani 1 1 d . . . 
N12 N 1.0372(7) 0.4317(6) 0.5827(9) 0.221(6) Uani 1 1 d . . . 
N13 N 0.1709(19) 0.4412(12) 0.458(2) 0.49(2) Uani 1 1 d DU . . 
O1 O 0.66057(19) 0.36670(14) 0.34525(19) 0.0614(8) Uani 1 1 d . . . 
O2 O 0.0874(4) 0.1893(4) 0.3313(5) 0.188(4) Uani 1 1 d . . . 
O3 O 0.7431(2) 0.44433(16) 0.4322(2) 0.0742(10) Uani 1 1 d . . . 
O5 O 0.1438(7) 0.2091(6) 0.4460(4) 0.267(6) Uani 1 1 d . . . 
O6 O 0.2060(6) 0.1705(6) 0.3593(13) 0.332(10) Uani 1 1 d . . . 
O7 O 0.6005(4) 0.4888(3) 0.1284(3) 0.144(3) Uani 1 1 d . . . 
H7B H 0.5795 0.4645 0.1463 0.216 Uiso 1 1 calc R . . 
O8 O 0.47996(17) 0.40903(14) 0.32949(17) 0.0580(8) Uani 1 1 d . . . 
O9 O 0.1786(8) 0.2432(7) 0.3455(10) 0.364(11) Uani 1 1 d . . . 
O1W O 0.7877(8) 0.2611(6) 0.5142(9) 0.154(5) Uani 0.50 1 d PU . . 
O2W O 0.5000 0.1506(13) 0.2500 0.220(14) Uani 0.50 2 d SPU . . 
O2WA O 0.418(3) 0.1509(12) 0.192(3) 0.21(2) Uani 0.25 1 d P . . 
O3W O 1.0000 0.4642(14) 0.2500 0.226(13) Uani 0.50 2 d SPU . . 
O3WA O 1.082(3) 0.451(2) 0.272(2) 0.26(3) Uani 0.25 1 d P . . 
 
 
_geom_special_details 
; 
 All esds (except the esd in the dihedral angle between two l.s. planes) 
 are estimated using the full covariance matrix.  The cell esds are taken 
 into account individually in the estimation of esds in distances, angles 
 and torsion angles; correlations between esds in cell parameters are only 
 used when they are defined by crystal symmetry.  An approximate (isotropic) 
 treatment of cell esds is used for estimating esds involving l.s. planes. 
; 
 
loop_ 
 _geom_bond_atom_site_label_1 
 _geom_bond_atom_site_label_2 
 _geom_bond_distance 
 _geom_bond_site_symmetry_2 
 _geom_bond_publ_flag 
Ni1 N1 2.078(4) 2_655 ? 
Ni1 N1 2.078(4) . ? 
Ni1 O8 2.083(3) . ? 
Ni1 O8 2.083(3) 2_655 ? 
Ni1 N4 2.113(4) 2_655 ? 
Ni1 N4 2.113(4) . ? 
Cl1 O9 1.259(9) . ? 
Cl1 O6 1.281(10) . ? 
Cl1 O5 1.304(8) . ? 
Cl1 O2 1.441(7) . ? 
Ni2 O1 1.819(4) . ? 
Ni2 N3 1.844(5) . ? 
Ni2 N5 1.861(5) . ? 
Ni2 N11 1.890(5) . ? 
Ni3 O3 2.028(4) . ? 
Ni3 N2 2.032(4) . ? 
Ni3 O1 2.038(3) . ? 
Ni3 N10 2.091(5) . ? 
Ni3 N7 2.105(4) . ? 
Ni3 N8 2.121(4) . ? 
C1 N1 1.311(6) . ? 
C1 N3 1.330(6) . ? 
C1 C2 1.487(7) . ? 
C2 N4 1.360(7) . ? 
C2 C7 1.365(7) . ? 
C3 N2 1.288(6) . ? 
C3 N9 1.369(7) . ? 
C3 C15 1.479(7) . ? 
C5 N4 1.316(7) . ? 
C5 C6 1.358(8) . ? 
C5 H5A 0.9300 . ? 
C6 C8 1.345(10) . ? 
C6 H6C 0.9300 . ? 
C7 C8 1.390(9) . ? 
C7 H7A 0.9300 . ? 
C8 H8A 0.9300 . ? 
C9 C10 1.338(9) . ? 
C9 N11 1.344(8) . ? 
C9 H9C 0.9300 . ? 
C10 C11 1.409(11) . ? 
C10 H10B 0.9300 . ? 
C11 C12 1.344(11) . ? 
C11 H11A 0.9300 . ? 
C12 C13 1.373(8) . ? 
C12 H12A 0.9300 . ? 
C13 N11 1.365(8) . ? 
C13 C14 1.455(9) . ? 
C14 N5 1.291(7) . ? 
C14 N6 1.356(8) . ? 
C15 N7 1.355(7) . ? 
C15 C16 1.377(7) . ? 
C16 C17 1.363(10) . ? 
C16 H16A 0.9300 . ? 
C17 C18 1.360(11) . ? 
C17 H17A 0.9300 . ? 
C18 C19 1.389(10) . ? 
C18 H18A 0.9300 . ? 
C19 N7 1.329(7) . ? 
C19 H19A 0.9300 . ? 
C20 C21 1.377(9) . ? 
C20 N10 1.403(8) . ? 
C20 H20A 0.9700 . ? 
C20 H20B 0.9700 . ? 
C21 N8 1.450(8) . ? 
C21 H21A 0.9700 . ? 
C21 H21B 0.9700 . ? 
C22 N8 1.457(7) . ? 
C22 C23 1.494(8) . ? 
C22 H22A 0.9700 . ? 
C22 H22B 0.9700 . ? 
C23 O7 1.347(9) . ? 
C23 H23A 0.9700 . ? 
C23 H23B 0.9700 . ? 
C29 N12 1.102(16) . ? 
C29 C30 1.47(2) . ? 
C31 C32 1.434(8) . ? 
C31 H31A 0.9600 . ? 
C31 H31B 0.9600 . ? 
C31 H31C 0.9600 . ? 
C32 N13 1.115(8) . ? 
N1 O1 1.409(5) . ? 
N2 O8 1.362(5) . ? 
N3 H3A 0.8600 . ? 
N5 O3 1.337(6) . ? 
N6 H6A 0.8600 . ? 
N6 H6B 0.8600 . ? 
N8 H8B 0.9100 . ? 
N9 H9A 0.8600 . ? 
N9 H9B 0.8600 . ? 
N10 H10A 0.9000 . ? 
N10 H10C 0.9000 . ? 
O7 H7B 0.8200 . ? 
O1W O1W 1.52(3) 7_656 ? 
O2W O2WA 1.69(6) . ? 
O2W O2WA 1.69(6) 2_655 ? 
O3W O3WA 1.56(6) 2_755 ? 
O3W O3WA 1.56(6) . ? 
 
loop_ 
 _geom_angle_atom_site_label_1 
 _geom_angle_atom_site_label_2 
 _geom_angle_atom_site_label_3 
 _geom_angle 
 _geom_angle_site_symmetry_1 
 _geom_angle_site_symmetry_3 
 _geom_angle_publ_flag 
N1 Ni1 N1 166.6(2) 2_655 . ? 
N1 Ni1 O8 90.50(15) 2_655 . ? 
N1 Ni1 O8 98.85(14) . . ? 
N1 Ni1 O8 98.85(14) 2_655 2_655 ? 
N1 Ni1 O8 90.50(15) . 2_655 ? 
O8 Ni1 O8 91.58(19) . 2_655 ? 
N1 Ni1 N4 76.84(16) 2_655 2_655 ? 
N1 Ni1 N4 93.45(16) . 2_655 ? 
O8 Ni1 N4 90.24(15) . 2_655 ? 
O8 Ni1 N4 175.34(14) 2_655 2_655 ? 
N1 Ni1 N4 93.45(16) 2_655 . ? 
N1 Ni1 N4 76.84(16) . . ? 
O8 Ni1 N4 175.34(14) . . ? 
O8 Ni1 N4 90.24(15) 2_655 . ? 
N4 Ni1 N4 88.3(2) 2_655 . ? 
O9 Cl1 O6 97.9(12) . . ? 
O9 Cl1 O5 113.9(12) . . ? 
O6 Cl1 O5 123.1(12) . . ? 
O9 Cl1 O2 106.7(7) . . ? 
O6 Cl1 O2 110.9(8) . . ? 
O5 Cl1 O2 103.7(7) . . ? 
O1 Ni2 N3 83.89(17) . . ? 
O1 Ni2 N5 91.17(17) . . ? 
N3 Ni2 N5 171.3(2) . . ? 
O1 Ni2 N11 172.84(18) . . ? 
N3 Ni2 N11 101.9(2) . . ? 
N5 Ni2 N11 83.6(2) . . ? 
O3 Ni3 N2 169.11(16) . . ? 
O3 Ni3 O1 86.63(14) . . ? 
N2 Ni3 O1 90.23(15) . . ? 
O3 Ni3 N10 87.78(19) . . ? 
N2 Ni3 N10 96.6(2) . . ? 
O1 Ni3 N10 170.62(18) . . ? 
O3 Ni3 N7 92.42(18) . . ? 
N2 Ni3 N7 77.53(17) . . ? 
O1 Ni3 N7 96.13(16) . . ? 
N10 Ni3 N7 91.62(17) . . ? 
O3 Ni3 N8 96.49(17) . . ? 
N2 Ni3 N8 93.94(16) . . ? 
O1 Ni3 N8 90.10(15) . . ? 
N10 Ni3 N8 83.05(17) . . ? 
N7 Ni3 N8 169.42(17) . . ? 
N1 C1 N3 120.7(5) . . ? 
N1 C1 C2 115.0(5) . . ? 
N3 C1 C2 124.3(4) . . ? 
N4 C2 C7 121.3(5) . . ? 
N4 C2 C1 114.5(4) . . ? 
C7 C2 C1 124.3(5) . . ? 
N2 C3 N9 123.2(5) . . ? 
N2 C3 C15 116.5(5) . . ? 
N9 C3 C15 120.2(5) . . ? 
N4 C5 C6 122.0(6) . . ? 
N4 C5 H5A 119.0 . . ? 
C6 C5 H5A 119.0 . . ? 
C8 C6 C5 120.7(6) . . ? 
C8 C6 H6C 119.7 . . ? 
C5 C6 H6C 119.7 . . ? 
C2 C7 C8 118.8(6) . . ? 
C2 C7 H7A 120.6 . . ? 
C8 C7 H7A 120.6 . . ? 
C6 C8 C7 118.5(6) . . ? 
C6 C8 H8A 120.8 . . ? 
C7 C8 H8A 120.8 . . ? 
C10 C9 N11 122.8(8) . . ? 
C10 C9 H9C 118.6 . . ? 
N11 C9 H9C 118.6 . . ? 
C9 C10 C11 118.3(7) . . ? 
C9 C10 H10B 120.9 . . ? 
C11 C10 H10B 120.9 . . ? 
C12 C11 C10 119.9(6) . . ? 
C12 C11 H11A 120.1 . . ? 
C10 C11 H11A 120.1 . . ? 
C11 C12 C13 119.5(7) . . ? 
C11 C12 H12A 120.3 . . ? 
C13 C12 H12A 120.3 . . ? 
N11 C13 C12 121.0(6) . . ? 
N11 C13 C14 112.5(5) . . ? 
C12 C13 C14 126.5(6) . . ? 
N5 C14 N6 123.3(6) . . ? 
N5 C14 C13 113.8(5) . . ? 
N6 C14 C13 122.7(6) . . ? 
N7 C15 C16 121.9(6) . . ? 
N7 C15 C3 113.2(4) . . ? 
C16 C15 C3 124.8(6) . . ? 
C17 C16 C15 118.9(7) . . ? 
C17 C16 H16A 120.6 . . ? 
C15 C16 H16A 120.6 . . ? 
C18 C17 C16 120.9(6) . . ? 
C18 C17 H17A 119.6 . . ? 
C16 C17 H17A 119.6 . . ? 
C17 C18 C19 117.0(7) . . ? 
C17 C18 H18A 121.5 . . ? 
C19 C18 H18A 121.5 . . ? 
N7 C19 C18 124.0(7) . . ? 
N7 C19 H19A 118.0 . . ? 
C18 C19 H19A 118.0 . . ? 
C21 C20 N10 120.4(7) . . ? 
C21 C20 H20A 107.2 . . ? 
N10 C20 H20A 107.2 . . ? 
C21 C20 H20B 107.2 . . ? 
N10 C20 H20B 107.2 . . ? 
H20A C20 H20B 106.9 . . ? 
C20 C21 N8 116.7(6) . . ? 
C20 C21 H21A 108.1 . . ? 
N8 C21 H21A 108.1 . . ? 
C20 C21 H21B 108.1 . . ? 
N8 C21 H21B 108.1 . . ? 
H21A C21 H21B 107.3 . . ? 
N8 C22 C23 118.9(6) . . ? 
N8 C22 H22A 107.6 . . ? 
C23 C22 H22A 107.6 . . ? 
N8 C22 H22B 107.6 . . ? 
C23 C22 H22B 107.6 . . ? 
H22A C22 H22B 107.0 . . ? 
O7 C23 C22 115.6(5) . . ? 
O7 C23 H23A 108.4 . . ? 
C22 C23 H23A 108.4 . . ? 
O7 C23 H23B 108.4 . . ? 
C22 C23 H23B 108.4 . . ? 
H23A C23 H23B 107.4 . . ? 
N12 C29 C30 175(2) . . ? 
C32 C31 H31A 109.5 . . ? 
C32 C31 H31B 109.5 . . ? 
H31A C31 H31B 109.5 . . ? 
C32 C31 H31C 109.5 . . ? 
H31A C31 H31C 109.5 . . ? 
H31B C31 H31C 109.5 . . ? 
N13 C32 C31 169(3) . . ? 
C1 N1 O1 108.7(4) . . ? 
C1 N1 Ni1 118.2(3) . . ? 
O1 N1 Ni1 133.1(3) . . ? 
C3 N2 O8 116.4(4) . . ? 
C3 N2 Ni3 117.5(3) . . ? 
O8 N2 Ni3 126.1(3) . . ? 
C1 N3 Ni2 111.1(3) . . ? 
C1 N3 H3A 124.5 . . ? 
Ni2 N3 H3A 124.5 . . ? 
C5 N4 C2 118.7(5) . . ? 
C5 N4 Ni1 125.8(4) . . ? 
C2 N4 Ni1 115.4(3) . . ? 
C14 N5 O3 117.3(5) . . ? 
C14 N5 Ni2 116.7(4) . . ? 
O3 N5 Ni2 125.9(3) . . ? 
C14 N6 H6A 120.0 . . ? 
C14 N6 H6B 120.0 . . ? 
H6A N6 H6B 120.0 . . ? 
C19 N7 C15 117.2(5) . . ? 
C19 N7 Ni3 128.3(5) . . ? 
C15 N7 Ni3 114.2(3) . . ? 
C21 N8 C22 111.8(6) . . ? 
C21 N8 Ni3 107.7(3) . . ? 
C22 N8 Ni3 115.4(4) . . ? 
C21 N8 H8B 107.2 . . ? 
C22 N8 H8B 107.2 . . ? 
Ni3 N8 H8B 107.2 . . ? 
C3 N9 H9A 120.0 . . ? 
C3 N9 H9B 120.0 . . ? 
H9A N9 H9B 120.0 . . ? 
C20 N10 Ni3 107.7(4) . . ? 
C20 N10 H10A 110.2 . . ? 
Ni3 N10 H10A 110.2 . . ? 
C20 N10 H10C 110.2 . . ? 
Ni3 N10 H10C 110.2 . . ? 
H10A N10 H10C 108.5 . . ? 
C9 N11 C13 118.5(5) . . ? 
C9 N11 Ni2 128.2(5) . . ? 
C13 N11 Ni2 113.3(4) . . ? 
N1 O1 Ni2 115.0(3) . . ? 
N1 O1 Ni3 122.8(3) . . ? 
Ni2 O1 Ni3 119.81(18) . . ? 
N5 O3 Ni3 115.7(3) . . ? 
C23 O7 H7B 109.5 . . ? 
N2 O8 Ni1 109.6(3) . . ? 
O2WA O2W O2WA 179(3) . 2_655 ? 
O3WA O3W O3WA 155(5) 2_755 . ? 
 
loop_ 
 _geom_torsion_atom_site_label_1 
 _geom_torsion_atom_site_label_2 
 _geom_torsion_atom_site_label_3 
 _geom_torsion_atom_site_label_4 
 _geom_torsion 
 _geom_torsion_site_symmetry_1 
 _geom_torsion_site_symmetry_2 
 _geom_torsion_site_symmetry_3 
 _geom_torsion_site_symmetry_4 
 _geom_torsion_publ_flag 
N1 C1 C2 N4 0.6(7) . . . . ? 
N3 C1 C2 N4 -179.0(5) . . . . ? 
N1 C1 C2 C7 179.4(6) . . . . ? 
N3 C1 C2 C7 -0.2(9) . . . . ? 
N4 C5 C6 C8 -0.3(12) . . . . ? 
N4 C2 C7 C8 2.0(10) . . . . ? 
C1 C2 C7 C8 -176.7(6) . . . . ? 
C5 C6 C8 C7 1.8(13) . . . . ? 
C2 C7 C8 C6 -2.6(12) . . . . ? 
N11 C9 C10 C11 -1.7(11) . . . . ? 
C9 C10 C11 C12 1.5(11) . . . . ? 
C10 C11 C12 C13 0.6(11) . . . . ? 
C11 C12 C13 N11 -2.5(10) . . . . ? 
C11 C12 C13 C14 178.2(6) . . . . ? 
N11 C13 C14 N5 -1.7(8) . . . . ? 
C12 C13 C14 N5 177.6(6) . . . . ? 
N11 C13 C14 N6 -177.9(6) . . . . ? 
C12 C13 C14 N6 1.4(10) . . . . ? 
N2 C3 C15 N7 -0.6(7) . . . . ? 
N9 C3 C15 N7 177.9(5) . . . . ? 
N2 C3 C15 C16 178.7(5) . . . . ? 
N9 C3 C15 C16 -2.9(9) . . . . ? 
N7 C15 C16 C17 -4.1(9) . . . . ? 
C3 C15 C16 C17 176.7(6) . . . . ? 
C15 C16 C17 C18 2.9(11) . . . . ? 
C16 C17 C18 C19 -0.2(11) . . . . ? 
C17 C18 C19 N7 -1.6(11) . . . . ? 
N10 C20 C21 N8 25.2(14) . . . . ? 
N8 C22 C23 O7 -55.6(10) . . . . ? 
N3 C1 N1 O1 -0.7(6) . . . . ? 
C2 C1 N1 O1 179.6(4) . . . . ? 
N3 C1 N1 Ni1 176.7(4) . . . . ? 
C2 C1 N1 Ni1 -3.0(6) . . . . ? 
N1 Ni1 N1 C1 47.5(4) 2_655 . . . ? 
O8 Ni1 N1 C1 -178.7(4) . . . . ? 
O8 Ni1 N1 C1 -87.0(4) 2_655 . . . ? 
N4 Ni1 N1 C1 90.5(4) 2_655 . . . ? 
N4 Ni1 N1 C1 3.1(4) . . . . ? 
N1 Ni1 N1 O1 -135.9(4) 2_655 . . . ? 
O8 Ni1 N1 O1 -2.1(4) . . . . ? 
O8 Ni1 N1 O1 89.5(4) 2_655 . . . ? 
N4 Ni1 N1 O1 -92.9(4) 2_655 . . . ? 
N4 Ni1 N1 O1 179.7(4) . . . . ? 
N9 C3 N2 O8 -4.9(7) . . . . ? 
C15 C3 N2 O8 173.5(4) . . . . ? 
N9 C3 N2 Ni3 174.5(4) . . . . ? 
C15 C3 N2 Ni3 -7.1(6) . . . . ? 
O3 Ni3 N2 C3 31.5(10) . . . . ? 
O1 Ni3 N2 C3 104.7(4) . . . . ? 
N10 Ni3 N2 C3 -81.8(4) . . . . ? 
N7 Ni3 N2 C3 8.5(4) . . . . ? 
N8 Ni3 N2 C3 -165.2(4) . . . . ? 
O3 Ni3 N2 O8 -149.1(7) . . . . ? 
O1 Ni3 N2 O8 -75.9(4) . . . . ? 
N10 Ni3 N2 O8 97.6(4) . . . . ? 
N7 Ni3 N2 O8 -172.2(4) . . . . ? 
N8 Ni3 N2 O8 14.2(4) . . . . ? 
N1 C1 N3 Ni2 -5.1(6) . . . . ? 
C2 C1 N3 Ni2 174.5(4) . . . . ? 
O1 Ni2 N3 C1 6.7(4) . . . . ? 
N5 Ni2 N3 C1 -49.1(15) . . . . ? 
N11 Ni2 N3 C1 -177.6(4) . . . . ? 
C6 C5 N4 C2 -0.4(9) . . . . ? 
C6 C5 N4 Ni1 175.6(5) . . . . ? 
C7 C2 N4 C5 -0.6(8) . . . . ? 
C1 C2 N4 C5 178.3(5) . . . . ? 
C7 C2 N4 Ni1 -176.9(5) . . . . ? 
C1 C2 N4 Ni1 1.9(6) . . . . ? 
N1 Ni1 N4 C5 10.6(5) 2_655 . . . ? 
N1 Ni1 N4 C5 -178.7(5) . . . . ? 
O8 Ni1 N4 C5 158.7(16) . . . . ? 
O8 Ni1 N4 C5 -88.2(4) 2_655 . . . ? 
N4 Ni1 N4 C5 87.3(4) 2_655 . . . ? 
N1 Ni1 N4 C2 -173.3(4) 2_655 . . . ? 
N1 Ni1 N4 C2 -2.6(3) . . . . ? 
O8 Ni1 N4 C2 -25(2) . . . . ? 
O8 Ni1 N4 C2 87.8(4) 2_655 . . . ? 
N4 Ni1 N4 C2 -96.6(4) 2_655 . . . ? 
N6 C14 N5 O3 0.3(9) . . . . ? 
C13 C14 N5 O3 -176.0(5) . . . . ? 
N6 C14 N5 Ni2 177.5(5) . . . . ? 
C13 C14 N5 Ni2 1.3(7) . . . . ? 
O1 Ni2 N5 C14 174.6(4) . . . . ? 
N3 Ni2 N5 C14 -130.0(12) . . . . ? 
N11 Ni2 N5 C14 -0.4(4) . . . . ? 
O1 Ni2 N5 O3 -8.4(4) . . . . ? 
N3 Ni2 N5 O3 47.0(15) . . . . ? 
N11 Ni2 N5 O3 176.5(4) . . . . ? 
C18 C19 N7 C15 0.5(9) . . . . ? 
C18 C19 N7 Ni3 173.8(5) . . . . ? 
C16 C15 N7 C19 2.4(8) . . . . ? 
C3 C15 N7 C19 -178.3(5) . . . . ? 
C16 C15 N7 Ni3 -171.8(5) . . . . ? 
C3 C15 N7 Ni3 7.5(6) . . . . ? 
O3 Ni3 N7 C19 2.3(5) . . . . ? 
N2 Ni3 N7 C19 178.1(5) . . . . ? 
O1 Ni3 N7 C19 89.2(5) . . . . ? 
N10 Ni3 N7 C19 -85.5(5) . . . . ? 
N8 Ni3 N7 C19 -145.1(8) . . . . ? 
O3 Ni3 N7 C15 175.8(4) . . . . ? 
N2 Ni3 N7 C15 -8.5(4) . . . . ? 
O1 Ni3 N7 C15 -97.4(4) . . . . ? 
N10 Ni3 N7 C15 87.9(4) . . . . ? 
N8 Ni3 N7 C15 28.4(11) . . . . ? 
C20 C21 N8 C22 -141.2(9) . . . . ? 
C20 C21 N8 Ni3 -13.4(10) . . . . ? 
C23 C22 N8 C21 -59.3(8) . . . . ? 
C23 C22 N8 Ni3 177.2(5) . . . . ? 
O3 Ni3 N8 C21 -85.7(5) . . . . ? 
N2 Ni3 N8 C21 97.4(5) . . . . ? 
O1 Ni3 N8 C21 -172.3(5) . . . . ? 
N10 Ni3 N8 C21 1.2(5) . . . . ? 
N7 Ni3 N8 C21 61.4(11) . . . . ? 
O3 Ni3 N8 C22 39.9(4) . . . . ? 
N2 Ni3 N8 C22 -136.9(4) . . . . ? 
O1 Ni3 N8 C22 -46.7(4) . . . . ? 
N10 Ni3 N8 C22 126.9(5) . . . . ? 
N7 Ni3 N8 C22 -172.9(8) . . . . ? 
C21 C20 N10 Ni3 -22.1(12) . . . . ? 
O3 Ni3 N10 C20 106.9(6) . . . . ? 
N2 Ni3 N10 C20 -83.1(6) . . . . ? 
O1 Ni3 N10 C20 53.5(14) . . . . ? 
N7 Ni3 N10 C20 -160.7(6) . . . . ? 
N8 Ni3 N10 C20 10.1(6) . . . . ? 
C10 C9 N11 C13 -0.2(10) . . . . ? 
C10 C9 N11 Ni2 -179.8(5) . . . . ? 
C12 C13 N11 C9 2.3(9) . . . . ? 
C14 C13 N11 C9 -178.3(5) . . . . ? 
C12 C13 N11 Ni2 -178.0(5) . . . . ? 
C14 C13 N11 Ni2 1.3(6) . . . . ? 
O1 Ni2 N11 C9 135.4(15) . . . . ? 
N3 Ni2 N11 C9 -7.9(6) . . . . ? 
N5 Ni2 N11 C9 179.0(6) . . . . ? 
O1 Ni2 N11 C13 -44.1(18) . . . . ? 
N3 Ni2 N11 C13 172.6(4) . . . . ? 
N5 Ni2 N11 C13 -0.6(4) . . . . ? 
C1 N1 O1 Ni2 6.4(5) . . . . ? 
Ni1 N1 O1 Ni2 -170.4(2) . . . . ? 
C1 N1 O1 Ni3 169.0(3) . . . . ? 
Ni1 N1 O1 Ni3 -7.9(6) . . . . ? 
N3 Ni2 O1 N1 -7.5(3) . . . . ? 
N5 Ni2 O1 N1 165.3(3) . . . . ? 
N11 Ni2 O1 N1 -151.4(15) . . . . ? 
N3 Ni2 O1 Ni3 -170.6(2) . . . . ? 
N5 Ni2 O1 Ni3 2.2(2) . . . . ? 
N11 Ni2 O1 Ni3 45.5(17) . . . . ? 
O3 Ni3 O1 N1 -160.1(3) . . . . ? 
N2 Ni3 O1 N1 30.3(3) . . . . ? 
N10 Ni3 O1 N1 -106.6(11) . . . . ? 
N7 Ni3 O1 N1 107.8(3) . . . . ? 
N8 Ni3 O1 N1 -63.7(3) . . . . ? 
O3 Ni3 O1 Ni2 1.6(2) . . . . ? 
N2 Ni3 O1 Ni2 -168.0(2) . . . . ? 
N10 Ni3 O1 Ni2 55.1(11) . . . . ? 
N7 Ni3 O1 Ni2 -90.5(2) . . . . ? 
N8 Ni3 O1 Ni2 98.1(2) . . . . ? 
C14 N5 O3 Ni3 -172.0(4) . . . . ? 
Ni2 N5 O3 Ni3 11.1(5) . . . . ? 
N2 Ni3 O3 N5 66.7(9) . . . . ? 
O1 Ni3 O3 N5 -6.7(3) . . . . ? 
N10 Ni3 O3 N5 -179.2(4) . . . . ? 
N7 Ni3 O3 N5 89.3(4) . . . . ? 
N8 Ni3 O3 N5 -96.4(3) . . . . ? 
C3 N2 O8 Ni1 -105.0(4) . . . . ? 
Ni3 N2 O8 Ni1 75.6(4) . . . . ? 
N1 Ni1 O8 N2 145.0(3) 2_655 . . . ? 
N1 Ni1 O8 N2 -25.4(3) . . . . ? 
O8 Ni1 O8 N2 -116.1(3) 2_655 . . . ? 
N4 Ni1 O8 N2 68.1(3) 2_655 . . . ? 
N4 Ni1 O8 N2 -3.2(19) . . . . ? 

_diffrn_measured_fraction_theta_max    0.968 
_diffrn_reflns_theta_full              27.48 
_diffrn_measured_fraction_theta_full   0.968 
_refine_diff_density_max    0.835 
_refine_diff_density_min   -0.695 
_refine_diff_density_rms    0.105 
